DOCSLIB.ORG

(12) Patent Application Publication (10) Pub. No.: US 2004/0171772 A1 Huffer Et Al

Total Page：16

File Type：pdf, Size：1020Kb

Download full-text PDF Read full-text
(12) Patent Application Publication (10) Pub. No.: US 2004/0171772 A1 Huffer Et Al US 2004.0171772A1 (19) United States (12) Patent Application Publication (10) Pub. No.: US 2004/0171772 A1 Huffer et al. (43) Pub. Date: Sep. 2, 2004 (54) METHOD FOR PRODUCING Publication Classification HOMOPOLYMERS AND COPOLYMERS OF ISOBUTENE (51) Int. Cl." ........................................................ C08F 2/00 (52) U.S. Cl. ............................ 526/64; 526/348.7; 526/82 (76) Inventors: Stephan Huffer, Ludwigshafen (DE); Hans Peter Rath, Grunstadt (DE); (57) ABSTRACT Gabriele Lang, Mannheim (DE); Jens Kremeskotter, Mannheim (DE); Elmar Homo- and copolymers of isobutene are prepared by con Stockelmann, Grunstadt (DE) tinuous cationic polymerization of isobutene or mixtures of isobutene with ethylenically unsaturated comonomers in the Correspondence Address: presence of an initiator System comprising: Nixon & Vanderhye i) a Lewis acid Selected from covalent metal-halogen 1100 North Glebe Road compounds and covalent Semimetal-halogen com Arlington, VA 22201-4714 (US) pounds and (21) Appl. No.: 10/476,701 ii) at least one aprotic organic compound I having at least one functional group FG which forms a car (22) PCT Filed: May 24, 2002 bocation or a cationic complex with the Lewis acid under polymerization conditions (86) PCT No.: PCT/EP02/05731 in an organic Solvent inert with respect to the Lewis acid, by (30) Foreign Application Priority Data a proceSS in which the polymerization is carried out in a tubular flow-through reactor which has a plurality of curves May 25, 2001 (DE)........................................ 101.25583.7 having an alternating direction of curvature. 1 3 Patent Application Publication Sep. 2, 2004 Sheet 1 of 5 US 2004/0171772 A1 Figure 1 : 3 3C Figure 2: Patent Application Publication Sep. 2, 2004 Sheet 2 of 5 US 2004/0171772 A1 Figure 3: O.:---- D2 Figure 4: Patent Application Publication Sep. 2, 2004 Sheet 4 of 5 US 2004/0171772 A1 Figure 6: 3 %O 6 3C US 2004/0171772 A1 Sep. 2, 2004 METHOD FOR PRODUCING HOMOPOLYMERS and copolymers of isobutene, it is an object of the present AND COPOLYMERS OF SOBUTENE invention to provide a continuous proceSS for the preparation of these polymers. 0001. The present invention relates to a continuous pro ceSS for the preparation of homo- and copolymers of 0008 We have found that this object is achieved, Sur isobutene by cationic polymerization of isobutene or mix prisingly, by polymerizing isobutene or mixtures of tures of isobutene with ethylenically unsaturated comono isobutene with ethylenically unsaturated comonomers con mers which copolymerize with isobutene under the condi tinuously in a helical tube reactor in the presence of an tions of a cationic polymerization. initiator System Suitable for the living cationic polymeriza tion. 0002 Polyisobutene and its copolymers are used in a variety of ways, for example for the preparation of fuel and 0009. The present invention thus relates to a process for lubricant additives, as elastomers, as adhesives for adhesive the preparation of homo- and copolymers of isobutene by raw materials, as a base component of Sealing and stopping continuous cationic polymerization of isobutene or mixtures compounds, in coating Systems, in particular those having a of isobutene with ethylenically unsaturated comonomers in barrier action for water vapor, and in chewing gum compo the presence of an initiator System comprising: Sitions. Block copolymers of isobutene with Vinylaromatic 0010 i) a Lewis acid selected from covalent metal monomers have, for example, elastomeric properties and halogen compounds and covalent Semimetal-halo high-gas tightness. gen compounds and 0003. The cationic polymerization of isobutene is fre 0011 ii) at least one aprotic organic compound I quently effected by boron trifluoride catalysis, in particular having at least one functional group FG which forms by polymerization of isobutene in the presence of boron a carbocation or a cationic complex with the Lewis trifluoride complex catalysts. Processes for this purpose acid under polymerization conditions have been described comprehensively in the prior art (cf. for 0012 in an organic solventinert with respect to the Lewis example DE-A 27 02 604, EP-A 145 235, EP-A 481 297, acid, wherein the polymerization is carried out in a helical EP-A 671. 419, EP-A 628 575, EP-A 807 641 and WO tube reactor. 99/31151). 0013 Helical tube reactors are disclosed in WO 0004 Kennedy et al. describe the homo- and copolymer 98/08602, which is hereby incorporated by reference for ization of isobutene under the conditions of a living cationic further details. A person skilled in the art understands a polymerization (cf. J. P. Kennedy et al. in U.S. Pat. No. helical tube reactor as meaning a curved, tubular flow 4,946,899, U.S. Pat. No. 4,327,201, U.S. Pat. No. 5,169,914, through reactor having a Substantially circular or ellipsoidal EP-A 206 756, EP-A 265 053 and comprehensively in J. P. (tube) croSS Section, wherein said reactor (or the reaction Kennedy, B. Ivan, Designed Polymers by Carbocationic tube) has a plurality of curves directly in Succession and Macromolecular Engineering, Oxford University Press, having an alternating direction of curvature. New York 1991). The initiator system used for the cationic 0014. The direction of curvature is reversed preferably no polymerization comprises, as a rule, at least one Lewis later than when that distance of the center of gravity of the acid-metal halide complex as a catalyst and at least one tube croSS-Sectional area which has been passed through organic compound which forms a carbocation or a cationic from the beginning of a curve is 200 times the tube diameter. complex with the Lewis acid under the reaction conditions. The curve may comprise up to three revolutions about the 0005 Although the living cationic polymerization leads axis of curvature. to polymerS having high molecular uniformity and more 0015. In the case of an ellipsoidal cross section of the over, in contrast to the boron trifluoride complex catalysis, also permits the Specific preparation of block copolymers reactor, tube diameter is understood as meaning the mean and of terminally functionalized polymers, it has only been value of major and minor axes. of academic importance to date. This is presumably due, on 0016 Curves having an alternating direction of curvature the one hand, to the fact that it is difficult to control and, on is to be understood here as meaning a Sequence of curved the other hand, to its high requirement with respect to the tube segments, the respective next tube segment (Section of purity of the reagents used. the tube between two Successive reversals of curvature, for example the Sections between two points of interSection of 0006 Because it is difficult to control, the living cationic axes in FIG. 1 to 4 of WO 98/08602) leading in a different polymerization is usually carried out as a batch process. The direction, preferably the opposite direction, to the preceding reaction vessels used are the Stirred kettles customary for one, i.e. there is a reversal of the direction of curvature with this purpose. In addition, the prior German patent applica each curved tube Segment. tions P10061715.8 and P10061727.1 propose the use of conventional, helically wound tubular reactors, as also used, 0017 Preferably, the reversal of the direction of curva for example, in the polymerization of isobutene underboron ture occurs no later than when that distance of the center of trifluoride catalysis, for a continuous embodiment of the gravity of the tube cross-sectional area which has been passed through from the beginning of a curve is 150, in proceSS. particular 100, preferably 80, particularly preferably 50, 30 0007. The Applicant's own experiments have shown that or 25, times the tube diameter. This distance is in general at the molecular uniformity of the polymers obtained by living least 5, in particular from 10 to 150, especially from 10 to cationic polymerization, in particular when the reaction is 100, preferably from 10 to 80, particularly preferably from carried out continuously, is unsatisfactory. Since the molecu 10 to 50, from 10 to 40 or from 10 to 30, times the tube lar uniformity is an important quality criterion for homo diameter. US 2004/0171772 A1 Sep. 2, 2004 0.018. A curve may comprise not only a partial revolution in the application, for example in the form of tubes or rods. but also one revolution or up to two or three revolutions In the case of a winding about 2 parallel axes, for example, about the axis of curvature. The angle covered by the normal the arrangement shown in FIGS. 1, 2 and 5 results. If a vector of the main direction of flow of a curve until a change winding is implemented about a plurality of axes preferably in the direction of curvature is thus in general s 10800, arranged in a plane, a band-like or wall-like design results, preferably s720°, particularly preferably s5 3600°. as shown in FIGS. 3 and 4. 0019. The curves are preferably substantially sinusoidal 0027 According to another preferred embodiment of the curves. In the present case, Sinusoidal curves are to be process, a helical tube reactor which is designed as a understood as meaning all types of, preferably periodically winding about a plurality of axes passing Substantially repeating, curves Substantially in a plane. The following through the Vertices of a polygon, in particular an equilateral description relates to the graph (Sinusoidal curve) described polygon, and perpendicular to its Surface is used. The by the path of the center of gravity of the tube diameter of polygon may have an even or, preferably, an uneven number the curved tube. The ratio of amplitude of curvature (greatest of vertices, in particular at least 3 or 5 and preferably 7, 9 or distance from the graph to a Straight line passing through 11 (cf.
Load more

Recommended publications
  • United States Patent Office Patented May 9, 1961 1
    2,983,583 United States Patent Office Patented May 9, 1961 1. 2 of the tube and drained into the hot Zone. Most of the 2,983,583 silicon tetrachloride was recovered unchanged. 0.43 millimole of BCls were obtained. Based on the SiCl4 METHOD OF PREPARNG BORON TRICHLORDE consumed, the yield of boron trichloride was about 70% FROM BORIC OXDE AND SILICON TETRA 5 based on Equation 2. CHLORDE Example III-In another experiment, conducted in William H. Schechter, Bradford Woods, Pa., assignor to a manner similar to those above, 10.0 millimoles of S2Cl2 Callery Chemical Company, Pittsburgh, Pa., a corpor was heated with 5.04 millimoles of BOs at 800° C. for ration of Pennsylvania 10 minutes. Boron trichloride and sulfur dioxide were O obtained in the volatile products, and a yellow solid, be No Drawing. Filed Mar. 28, 1958, Ser. No. 725,471 lieved to be sulfur, formed in the tube. 2 Claims. (CI. 23-205) Example IV.-9.32 millimoles of PC were passed over excess BO heated to 800° C. for 10 minutes. The vola This invention relates to the preparation of boron tri 15 tile products formed were analyzed with an infrared spec chloride and more particularly to the preparation of trometer and found to be predominantly BCl3. Some boron trichloride from boric oxide and non-metallic orange colored solids also formed in the reactor during chlorides. the reaction. The non-metallic chlorides which have been found Boron trichloride, BC, is used in several processes to useful in the practice of this invention are all volatile prepare other boron compounds, as a catalyst, and, in 20 liquids, at ordinary temperatures, and their reaction with general, is regarded as a basic boron compound.
    [Show full text]
  • Boron and Titanium(IV) Halide Mediated Reactions
    University of Tennessee, Knoxville TRACE: Tennessee Research and Creative Exchange Doctoral Dissertations Graduate School 8-2010 Boron and Titanium(IV) Halide Mediated Reactions Michael Patrick Quinn University of Tennessee - Knoxville, [email protected] Follow this and additional works at: https://trace.tennessee.edu/utk_graddiss Part of the Organic Chemistry Commons Recommended Citation Quinn, Michael Patrick, "Boron and Titanium(IV) Halide Mediated Reactions. " PhD diss., University of Tennessee, 2010. https://trace.tennessee.edu/utk_graddiss/908 This Dissertation is brought to you for free and open access by the Graduate School at TRACE: Tennessee Research and Creative Exchange. It has been accepted for inclusion in Doctoral Dissertations by an authorized administrator of TRACE: Tennessee Research and Creative Exchange. For more information, please contact [email protected]. To the Graduate Council: I am submitting herewith a dissertation written by Michael Patrick Quinn entitled "Boron and Titanium(IV) Halide Mediated Reactions." I have examined the final electronic copy of this dissertation for form and content and recommend that it be accepted in partial fulfillment of the requirements for the degree of Doctor of Philosophy, with a major in Chemistry. George W. Kabalka, Major Professor We have read this dissertation and recommend its acceptance: Shane Foister, Ziling (Ben) Xue, Paul Dalhaimer Accepted for the Council: Carolyn R. Hodges Vice Provost and Dean of the Graduate School (Original signatures are on file with official studentecor r ds.) To the Graduate Council: I am submitting herewith a dissertation written by Michael Patrick Quinn entitled ―Boron and Titanium(IV) Halide Mediated Reactions.‖ I have examined the final electronic copy of this dissertation for form and content and recommend that it be accepted in partial fulfillment of the requirements for the degree of Doctor of Philosophy, with a major in Chemistry.
    [Show full text]
  • Boron Trichloride. Bcl₃
    → Datasheet Boron trichloride. BCl₃ Product information BCl₃ is the main gas composition in High-K and metal anisotropic plasma etch. Atomic layer etch and pulsed plasma etch. BCl₃ is mainly used for fine etching of aluminum circuits in the manuf- acturing process of LCD panels. Characteristics Liquefied gas, decomposes in water to hydrogen chloride and boric acid. Forms white fumes in humid air. Pungent odor. Highly corrosive. Gas density is heavier than air. Physical data Molecular weight [g/mol] 117.17 Boiling point at 1.013 bar [°C] 12.5 at 14.5 psi [°F] 54.52 at 1.013 bar, Density 5.162 at 1 atm., 70 °F [lb/ft³] 0.315 15 °C [kg/m³] Vapor pressure at 0 °C [bar] 0.63 at 32 °F [psi] 9.09 at 20 °C [bar] 1.33 at 70 °F [psi] 19.91 Flammability range in air (% volume) Non-combustible Product specification Purity grade Typical purity Typical impurities [ppm] N₂ O₂+Ar CO CO₂ COCl₂ CH₄ HCl 5.0N ≥99.999 % ≤4 ≤1 ≤0.5 ≤1 ≤0.5 ≤0.5 ≤50 5.5N ≥99.99995 % ≤1 ≤0.5 ≤0.5 ≤1 ≤0.5 ≤0.5 ≤25 Contact our team for higher grade or different specification products. Shipping information UN number CAS number EC number DOT label Hazard labels required 1741 10294-34-5 233-658-4 Poison gas ADR Class 2, 2 TC DOT Class 2.3 → Boron trichloride. Product datasheet. Page 2 Packaging information Package Cylinder Cylinder Cylinder Cylinder Cylinder Cylinder Fill Pressure Valve Valve designa- internal material diameter height to tare weight contents (psig) outlet material options o tion volume valve outlet @ 70 F US Cylinder 209 44 L Nickel 9 in 52 in 130 lb 110 lb 4.4 CGA
    [Show full text]
  • Chemical Names and CAS Numbers Final
    Chemical Abstract Chemical Formula Chemical Name Service (CAS) Number C3H8O 1‐propanol C4H7BrO2 2‐bromobutyric acid 80‐58‐0 GeH3COOH 2‐germaacetic acid C4H10 2‐methylpropane 75‐28‐5 C3H8O 2‐propanol 67‐63‐0 C6H10O3 4‐acetylbutyric acid 448671 C4H7BrO2 4‐bromobutyric acid 2623‐87‐2 CH3CHO acetaldehyde CH3CONH2 acetamide C8H9NO2 acetaminophen 103‐90‐2 − C2H3O2 acetate ion − CH3COO acetate ion C2H4O2 acetic acid 64‐19‐7 CH3COOH acetic acid (CH3)2CO acetone CH3COCl acetyl chloride C2H2 acetylene 74‐86‐2 HCCH acetylene C9H8O4 acetylsalicylic acid 50‐78‐2 H2C(CH)CN acrylonitrile C3H7NO2 Ala C3H7NO2 alanine 56‐41‐7 NaAlSi3O3 albite AlSb aluminium antimonide 25152‐52‐7 AlAs aluminium arsenide 22831‐42‐1 AlBO2 aluminium borate 61279‐70‐7 AlBO aluminium boron oxide 12041‐48‐4 AlBr3 aluminium bromide 7727‐15‐3 AlBr3•6H2O aluminium bromide hexahydrate 2149397 AlCl4Cs aluminium caesium tetrachloride 17992‐03‐9 AlCl3 aluminium chloride (anhydrous) 7446‐70‐0 AlCl3•6H2O aluminium chloride hexahydrate 7784‐13‐6 AlClO aluminium chloride oxide 13596‐11‐7 AlB2 aluminium diboride 12041‐50‐8 AlF2 aluminium difluoride 13569‐23‐8 AlF2O aluminium difluoride oxide 38344‐66‐0 AlB12 aluminium dodecaboride 12041‐54‐2 Al2F6 aluminium fluoride 17949‐86‐9 AlF3 aluminium fluoride 7784‐18‐1 Al(CHO2)3 aluminium formate 7360‐53‐4 1 of 75 Chemical Abstract Chemical Formula Chemical Name Service (CAS) Number Al(OH)3 aluminium hydroxide 21645‐51‐2 Al2I6 aluminium iodide 18898‐35‐6 AlI3 aluminium iodide 7784‐23‐8 AlBr aluminium monobromide 22359‐97‐3 AlCl aluminium monochloride
    [Show full text]
  • Heat of Formation of Boron Trichloride Walter H
    Journal of Research of the National Bureau of Sta nda rds Vol. 62, No.5, May 1959 Research Paper 2956 Heat of Formation of Boron Trichloride Walter H. Johnson, Richard G . Miller, ! a nd Edward J. Prosen The heat of formation of gaseou boron t richloride has been determined by t he direct reaction of gaseous chlorine with amorphous boron in a calorimeter. B (amorph) + 3/2 CIz (gas) = BCh(gas) AHfO(25° C)= - 407.98 ± 1.34 kj/mole (- 97.51 ± 0.32 kcal/moJe). By utilizing t he valu es previously reported for the hea ts of formation of boric acid, dibor­ ane, and pentaborane, t he heat of hydrolysis of boron t richloride and the heats of reac­ tion of dibora ne a nd pentaboran e wit h chlorine have been obtained. By the use of an estimat ed value for t he heat of sublimation of boron, the average bond energy of t he B- CI bond in boron t richloride is found to be 105. 2 k cal at 0° K . The data on the heats of formation of diborane, boric oxide, boric acid, and boron trichloride now form a co n­ sistent set of values. I. Introduction 3. Materials and Apparatus The heat of formation of boron trichloride has The boron was prepared by the thermal de compo­ long been uncertain because of the fact that calcu­ sition of diborane by pa sing diborane diluted with lation of it has been dependent upon uncertain values helium through a quartz tube heated to 600 0 C [1] .
    [Show full text]
  • Oom O#00Noo-O
    March 9, 1943. H, wALTHER 2,313,410 PREPARATION OF BORON COMPOSITIONS Filéd March 31, 1959 O00NoO-OomOO# SWHO Nl SQNVLS/SSH .7/dl33d5 /N VE/V TOR H. WAL THER BV mgm ATTORNEY Patented Mar. 9, 1943 2,313,410 UNITED STATES PATENT OFFICE 2,313,410 PREPARATION 0F BORON COMPOSITIONS Henry Walther, Millburn, N. J., assignor to Beil Telephone Laboratories, Incorporated, New York, N. Y., a cgrporation of New York Application March 31, 1939, Serial No. 265,183 14 Claims. (Cl. 117-107) This invention relates to the preparation of tallic halide combines with the hydrogen in the resistor elements which have a negative tem proximity of the filament to deposit the metal perature coefllcient of resistance and more par thereon simultaneously with the formation of ticularly to the preparation of boron thermistors. the boron. The resulting product is homoge An object of this invention is to modify a mass neous and the ñlament upon which the boron of boron to change the characteristics thereof for and metal is deposited serves as a convenient rendering it suitable for use as a thermistor. guide for securing a required length of resist Another object of this invention is to incor ance unit. Alternatively, other metals or silicon porate throughout a mass of boron homogeneous or nitrogen may be incorporated with the boron ly another element. ‘ ~ ¿ 10 by subjecting boron trichloride, a reducing me A more particular object of this invention is dium and elemental nitrogen or a vaporized com to prepare simultaneously boron and another ele pound of the metal or silicon, such as a metal ment to produce a homogeneous substance adapt lic halide or silicon tetrachloride, to a heated sur ed for use as a thermistor.
    [Show full text]
  • R Ysssssssss
    Nov. 5, 1957 w A. R. GLOBUS 2,812,240 PROCESS OF MAKING BORON NITRIDE Filed Feb. 17, 1955 sS s : r N 1 - a 4th 8 R ... SNs S. s INVENTOR SSat man avia as a awarar ar.Kettes. N N: aAAAACsy A, GZOAAS NA s : RN A... 6 YSSSSSSSSSa gram ATTORNEY 2,812,240 United States Patent Office Patented Nov. 5, 1957 2 through valvcd pipe 39 to pump 41, by which the mixture 2,812,240 is forced through pipe 42 and vertical section 43 back inio the lower end of reactor . Heat is supplied by PROCESS OF MAKING BORON NITRIDE In eans of the elix 45 to keep the vertical section 43 at Alfed R. Globus, Forest Hills, N. Y., assignor to United a temperature above the melting point of the metal. ternational Research, Inc., a corporation of New The nitrogen introduced with the boron trichloride should be at least Sioichiometrically sufficient to react York with the horon prescrlt in the trichloride, with formation Application February 17, 1955, Serial No. 488,920 of boron nitride (BN). In practice a substantial excess 1 Claim. (C. 23-191) O of nitrogen will he used to insure completion of the de sired reaction and the maintenance cf a nitrogen atmos This invention is a new and useful process of making phere in the free space in the upper cnd of reactor 1. boron nitride and will be fully understood from the fol The boron trichloride will react immediately with the lowing description read in conjunction with the drawing allininum, with production of aluminum chloride (AlCl3) in which: and boron, which boron reacts immediately with the Fig.
    [Show full text]
  • THE MONATOMIC IONS! 1. What Is the Formula for Silver? Ag 2. What Is
    Name: ______________________________ THE MONATOMIC IONS! 1. What is the formula for silver? Ag+ 22. What is the formula for cobalt (II)? Co2+ 2. What is the formula for cadmium? Cd2+ 23. What is the formula for chromium (II)? Cr2+ 3. What is the formula for manganese (II)? Mn2+ 24. What is the formula for copper (II)? Cu2+ 4. What is the formula for nickel (II)? Ni2+ 25. What is the formula for tin (IV)? Sn4+ 5. What is the formula for chromous? Cr2+ 26. What is the formula for lead (IV)? Pb4+ 6. What is the formula for zinc? Zn2+ 27. What is the formula for iron (III)? Fe3+ 2+ 2+ 7. What is the formula for cobaltous? Co 28. What is the formula for mercury (I)? Hg2 8. What is the formula for cuprous? Cu+ 29. What is the formula for lead (II)? Pb2+ 9. What is the formula for ferrous? Fe2+ 30. What is the formula for mercury (II)? Hg2+ 2+ 2+ 10. What is the formula for mercurous? Hg2 31. What is the formula for iron (II)? Fe 11. What is the formula for stannous? Sn2+ 32. What is the formula for copper (I)? Cu+ 12. What is the formula for plumbous? Pb2+ 33. What is the formula for tin (II)? Sn2+ 13. What is the formula for chromic? Cr3+ 34. What is the formula for fluoride? F- 14. What is the formula for cobaltic? Co3+ 35. What is the formula for chloride? Cl- 15. What is the formula for cupric? Cu2+ 36. What is the formula for hydride? H- 16.
    [Show full text]
  • A New Multifunctional Initiator System for the Living Cationic Polymerization of Vinyl Ethers
    472 Macromol. Rapid Commun. 21, 472–475 (2000) Communication: Combination of hexa(chloromethyl)- melamine (HCMM) and zinc chloride was found to be a multifunctional initiator system for the living cationic polymerization of isobutyl vinyl ether. HCMM was synthe- sized by reaction of hexa(methoxymethyl)melamine and boron trichloride. Characterization of the polymers by means of GPC and 1H NMR showed that initiation was rapid and quantitative and that the initiator is hexafunc- tional, leading to six-armed star-shaped polymers. A new multifunctional initiator system for the living cationic polymerization of vinyl ethers Xiaochun Zhang1, Eric J. Goethals*1, Ton Loontjens2, Frank Derks2 1 University of Gent, Department of Organic Chemistry, Polymer Chemistry Division, Krijgslaan 281(S4-bis), 9000 Gent, Belgium 2 DSM Research, P.O. Box, 6160 MD Geleen, The Netherlands (Received: January 19, 2000) Introduction diethyl ether (1.0 M) and BCl3 in hexane (1.0 M) were pur- chased from Aldrich and used without further treatment. For the synthesis of star-shaped polymers, two methods Hexa(methoxymethyl)melamine (HMMM) (Cymel 303) was 1–3) based on living polymerization have been described : purchased from American Cynamide and used without end-capping of linear living polymers with a multifunc- further purification. tional end-capper (“arm-first” method), and initiation of the polymerization with a multifunctional initiator system (“core-first” method). In case of living cationic polymeri- Synthesis of hexa(chloromethyl)melamine (HCMM) zation of vinyl ethers, star-shaped polymers have been A 250 ml double-cocked flask provided with rubber septum prepared by both methods4, 5). The core-first method has and magnetic stirring bar containing 4.0 g of HMMM was the advantage that, at the end of the polymerization, end- dried in vacuum at 408C for 1 h and then filled with dry capping of the living chain ends is still possible, thus pro- argon.
    [Show full text]
  • Boron Trichloride
    Material Safety Data Sheet 1. Product and Company Identification Product name : Boron Trichloride Chemical formula : BCl3 Synonyms : Trichloroborane Company : Specialty Gases of America, Inc 6055 Brent Dr. Toledo, OH 43611 Telephone : 419-729-7732 Emergency : 800-424-9300 2. Composition/Information on Ingredients Components CAS Number % Volume Boron Trichloride 10294-34-5 100% 3. Hazards Identification Emergency Overview Colorless poison gas with acidic odor. Nonflammable. Irritating and corrosive to the eyes, skin and respiratory system. Exposure to high concentrations may result in burns to mucous membranes. Inhalation into the deep lung may result in dangerous retention of body fluid and swelling in the lungs (pulmonary edema) and chemical pneumonitis. Hydrolyzes into hydrochloric and boric acid in the presence of water or moisture. Contents under pressure. Use and store below 125 F. Potential Health Effects Inhalation : Boron trichloride hydrolyzes very rapidly into hydrochloric acid and boric acid in the presence of moisture. Slight exposure results in irritation of the upper respiratory tract and cough. Higher concentrations may cause inflammation and congestion of the lungs. Inhalation into the deep lung may result in difficulty breathing, chest pain, chemical pneumonitis and fluid retention with swelling in the lungs (edema). May cause shock, coma and death. Eye contact : Eye contact will cause severe irritation, inflammation, and painful burns. Burns may result in lesions and blindness. PERSONS WITH POTENTIAL EXPOSURE TO BORON TRICHLORIDE SHOULD NOT WEAR CONTACT LENSES. Skin contact : Low concentrations may cause “stinging” of the skin. Severe burns may result at higher concentrations. Inorganic acid-like burns and corrosive action will occur at high concentrations resulting in lesions and early necrosis.
    [Show full text]
  • Preparation of Diborane from Lithium Hydride and Boron Trihalide Ether Complexes1
    OCt. 20, 1952 &BORANE FROM LITHIUMHYDRIDE AND BORONTRIHALIDE ETHER COMPLEXES 5047 [CONTRIBUTION FROM THE RESEARCH LABORATORYOF THE GENERALELECTRIC COMPANY] Preparation of Diborane from Lithium Hydride and Boron Trihalide Ether Complexes1 BY J. R. ELLIOTT,E. M. BOLDEBUCKAND G. F. ROEDEL RECEIVEDFEBRUARY 14, 1952 The preparation of diborane from lithium hydride and boron trihalide etherates under different conditions is described and secondary reactions are discussed. The reaction between lithium hydride and boron trifluoride in ethyl ether has been shown to proceed by two different courses. If ether-soluble, active hydrogen-containing promoters are present, or if pressure is used to force the reaction between lithium hydride and diborane, the hydride is converted completely to lithium borohydride and lithium fluoride before diborane is evolved. In the absence of soluble promoters, diborane escapes continually from the solution, lithium borofluoride is formed and lithium borohydride does not accumulate. If less than a specified ratio of boro- hydride to hydride exists in the ether solution, the borohydride is consumed in the continuing reaction, and diborane is evolved. In tetrahydrofuran, a promoter is not required for the conversion of lithium hydride to lithium borohydride. Since the solubility of diborane is relatively high in tetrahydrofuran, conditions favor the production of borohydride by reaction of diborane with lithium hydride, as in the pressure reaction with ether as solvent. Introduction continuously evolved at a mole rate
    [Show full text]
  • Boron Trichloride Safety Data Sheet
    Boron trichloride Safety Data Sheet P-4566 This SDS conforms to U.S. Code of Federal Regulations 29 CFR 1910.1200, Hazard Communication. Issue date: 01/01/1979 Revision date: 01/21/2021 Supersedes: 10/13/2016 Version: 1.0 SECTION: 1. Product and company identification 1.1. Product identifier Product form : Substance Substance name : Boron trichloride CAS-No. : 10294-34-5 Formula : BCl3 1.2. Relevant identified uses of the substance or mixture and uses advised against Use of the substance/mixture : Industrial use; Use as directed. 1.3. Details of the supplier of the safety data sheet Linde Inc. 10 Riverview Drive Danbury, CT 06810-6268 - USA www.lindeus.com Linde Inc. 1-844-44LINDE (1-844-445-4633) Linde Electronics 1-800-932-0624 or 1-908-329-9700 1.4. Emergency telephone number Emergency number : Onsite Emergency: 1-800-645-4633 CHEMTREC, 24hr/day 7days/week — Within USA: 1-800-424-9300, Outside USA: 001-703-527-3887 (collect calls accepted, Contract 17729) SECTION 2: Hazard identification 2.1. Classification of the substance or mixture GHS US classification Press. Gas (Liq.) H280 Acute Tox. 3 (Inhalation:gas) H331 Skin Corr. 1B H314 Eye Dam. 1 H318 STOT SE 3 H335 2.2. Label elements GHS US labeling Hazard pictograms (GHS US) : GHS04 GHS05 GHS06 Signal word (GHS US) : Danger Hazard statements (GHS US) : H280 - CONTAINS GAS UNDER PRESSURE; MAY EXPLODE IF HEATED H314 - CAUSES SEVERE SKIN BURNS AND EYE DAMAGE H331 - TOXIC IF INHALED CGA-HG22 - CORROSIVE TO THE RESPIRATORY TRACT CGA-HG01 - MAY CAUSE FROSTBITE.
    [Show full text]