IL45558A - Thermoplastic polivinylchloride composition - Google Patents
Thermoplastic polivinylchloride compositionInfo
- Publication number
- IL45558A IL45558A IL45558A IL4555874A IL45558A IL 45558 A IL45558 A IL 45558A IL 45558 A IL45558 A IL 45558A IL 4555874 A IL4555874 A IL 4555874A IL 45558 A IL45558 A IL 45558A
- Authority
- IL
- Israel
- Prior art keywords
- weight
- polyethylene
- thermoplastic composition
- chlorination
- low pressure
- Prior art date
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/18—Introducing halogen atoms or halogen-containing groups
- C08F8/20—Halogenation
- C08F8/22—Halogenation by reaction with free halogens
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/26—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment
- C08L23/28—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment by reaction with halogens or compounds containing halogen
- C08L23/286—Chlorinated polyethylene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Description
45558/2 THERMOPLASTIC POLIVINYLCHLORIDE COMPOSITION This invention relates to a thermoplastic composition con^ sisting of a vinyl chloride polymer and a. chlorinated low pressure polyethylene.
It has been proposed to elastify polyvinyl chloride and vinyl chloride copolymers by the addition of chlorination products of polyolefins obtained by chlorinating polyolefins in aqueous suspension and having a chlorine content of from 25 to 50 io by weight (cf. German Patent 1, ¾69 , 990 and German Patents 1, 23 , 77¾ and 1, 266 , 969 ) .
To obtain chlorination products having a good elastifying effect combined with a sufficient fineness of grain the chlorination has to be carried out in the presence of fine-grained inert, inorganic or organic additives to avoid agglomeration. As inorganic additives silicic acid or kieselguhr have been proposed (cf. German Patent 1, ¾20 , ¾07 ) .
The relatively large amount of silicic acid, wh¾.h must be added to the chirination reaction as anti-agglomeration agent and which partially remains in the final blend when the chloro-polyolefin is mixed with polyvinyl chloride, has a detrimental effect on the Theological and mechanical properties of the blend.
It has now been found that mixtures of vinyl chloride polymers and chlorination products of polyolefins can be produced which do^iot have the aforesaid disadvantages and are well suitable for dry blend technique by using a chlorinated low pressure polyethylene prepared by chlorinating in aqueous hydrochloric acid, preferably in the presence of silicic acid having a large surface and a siloxane oil.
The present invention provides a thermoplastic composition essentially consisting of* a) 8 to 50 Ί° by weight of* a vinyl chloride polymer and b) 2 to 5° $ by weight of a chlorinated low pressure polyethylene, having a chlorine content of" 25 to 2 $ by weight, a reduced specific viscosity of 1 to dl/g» a residue value of 2 to 4θ measured by extraction with toluene/ acetone in a proportion of 1 : 1 , and a swelling value of 10 to 70 measured in methylcyclohexane, and obtained by chlorinating a low pressure polyethylene in aqueous hydrochloric acid having a strength of from 10 to 35 preferably 1 5 to 30 ia in the presence of 0 to 2 by weight of silicic acid and 0 to 1 .0 $ by weight of a siloxane oil, the percentages being calculated on the low pressure polyethylene used, at a chlorination temperature of from 50 to 130°C, at least 10 by weight of chlorine being incorporated at a temperature of from 1 20 to 1 30°C.
The present invention also provides a process for the manufacture of a thermoplastic composition by mixing a) 98 to 50 ^ by weight of a vinyl chloride polymer and b) 2 to 0 70 by weight of a chlorinated low pressure polyethylene having a chlorine content of from 25 to 42 $ by weight, a reduced specific viscosity of 1 to 5 dl/g> a residue value of from 2 to 40 7¾, measured by extraction with toluene/acetone in a proportion of 1 : 1 , and a swelling value of from 10 to 70 measured in methylcyclohexane, prepared by chlorinating a preferably fine-grained low pressure polyethylene in aqueous hydrochloric acid of 10 to 35 preferably 1 5 to 30 strength in the presence of 0 to 2 by weight of silicic acid and 0 to 1 .0$ by weight of a siloxane oil, the percentages being calculated on the starting polyethylene, at a chlorination temperature of from 50 to 1 30°C, the low pressure polyethylene being possibly thermally treated or presintered at a temperature in the range of from 1 00°C to ±bs crystallite melting point and at least 10 70 of the chlorine being incorporated at a temperature of from 1 20 to 1 30°C.
The thermoplastic composition consists of 98 to 50 $ y weight, preferably 95 to 80 7° y weight, of polyvinyl chloride or a copolymer of vinyl chloride with other comonomers , such as vinyl acetate, acrylic acid esters or methacrylic acid esters, the amount of comonomer units in the polymer being at most 20 70 by weight, preferably 1 to 70 by weight. The K value of the polymer is expediently in a range of from 50 to 80.
The remaining 2 to 50 70 by weight, preferably 2 to 20 by weight of the thermoplastic composition of the invention consists of a chlorinated low pressure polyethylene of high molecular weight containing 25 to 2 70 by weight, preferably 30 to kO by weight, of chlorine. The distribution of the chlorine atones in the polyethylene grains, i.e. the degree of "penetrating or through chlorination" is characterized by the residue value according to the toluene/acetone method and the swelling value in methylcyclohexane . The chlorinated low pressure polyethylene suitable for making the compositions of the invention shall have a residue value of 2 to kO $>, preferably 2 to 30 70, and a swelling value of 1 0 to 70 70, preferably 20 to 0 Moreover, it shall have a reduced specific viscosity of 1 to 5 preferably 1 to 3 . 5 dl/g.
The chlorinated low pressure polyethylene of high molecular - k - eight is fine-grained and can readily be mixed homogeneously^ with the vinyl chloride polymer powder.
The chlorinated low pressure polyethylene to be used according to the invention is produced by chlorinating finegrained low pressure polyethylene, which may have been thermally treated or pre-sintered for 5 to 300 minutes at a temperature of from 100°C to its crystallite melting point (cf. German Offenlegungsschrift 1 , 720,800), in hydrochloric acid^ expedi- i ently 3 to 30 times the amount of acid is used, referred to the low pressure polyethylene. The chlorination is started at a temperature of from 50 to 100°C and terminated at 120 to 1 30°C.
The chlorination is advantageously started in a temperature range of from 70 to 90°C, continued with continual temperature increase and terminated at a temperature ranging from 1 20 to 1 30°C. Alternatively, the chlorination can be effected in two steps, i.e. it is started at a temperature of from 50°C to 100°C, the chlorine supply is interrupted while the temperature is raised to 1 20 to 1 30°C and the chlorination is then continued and terminated at that temperature.
The low pressure polyethylene used as starting material has a reduced specific viscosity of 1 to 5 dl/g» preferably 1 to 3. 5 dl/g.
By silicic acid present in the chlorination as agglomeration inhibitor the various hydrous or anhydrous types of finely porous silicon dioxide preferably having a large surface are understood. Their inner surface should expediently be in the range of from 50 to hOO cm /g according to BET (Brunauer, 2 Emmet and Teller), preferably 1 0 to 300 cm /g.
In general the silicic acid has a mean particle size of from 1 to 50 yum.
By the addition of silicic acid and siloxane oil the anti-agglomeration effect of hydrochloric acid is improved.
Such an addition is therefore preferred. Xn general 0. 1 to 2 preferably 0. 1 to 1 $ by weight of silicic acid in combination with 0. 01 to 1 . 0 , preferably 0.02 to 0.7 by weight, of siloxane oil, each time calculated on the low pressure polyethylene used, are sufficient. The amount of silicic acid and siloxane oil is not strictly limited, in some cases higher amounts may also be used, whereby the agglomeration inhibition is further improved but disadvantages for the blend with polyvinyl chloride must be taken into consideration.
The organo-silicon compounds or siloxane oils to be used according to the invention are liquid polysiloxanes consisting of the recurring unit in which and each represents an alkyl radical preferably having from 1 to 6 carbon atoms, an aryl radical , preferably a phenyl or an aralkyl radical preferably having from 7 to 12 carbon atoms, and X is an integer of from 10> to 1 , 000. he viscosity of the siloxane oils at 25° C is suitably in the range of from to 500 , 000 centistokes, more suitably 500 to 50 , 000 centi-stokes. There are mentioned, by way of example, dimethyl-, diethyl-, dipropyl-, methyl-ethyl-, dioctyl-, dihexyl-, methyl propyl-, dibutyl- and didodecyl-polysiloxanes * Compounds of the dimethyl-polysiloxane series proved to be especially ad- vantageous.
The silicic acid component and the polysiloxane , which are possibly pre-mixed, are expediently added prior to or at the beginning of the chlorination within a temperature interval in which the melting point of the polyethylene is not yet reached.
According to another mode of operation the silicic acid is first added alone and the siloxane oil is then admixed during the course of chlorination. A possible slight agglomeration can be counter-acted at least partially by the later addition of siloxane oil, even if it Is made prior to drying.
It is also possible, of course, to add the intended amount i of siloxane oil in portions during some or all process steps.
The thermoplastic composition according to the invention may additionally contain known PVC stabilizers, for example barium or cadmium laurate, epoxide stabilizers, organic phosphites, tin or lead compounds, as well as other known additives, for example UV absorbers, lubricants, processing auxiliaries, dyes and pigments.
Depending on the proportion of chlorinated low pressure polyethylene, the thermoplastic composition of the invention can be used for making pipes, profiles, plates, sheets, cables, flexible tubes, injection moulded articles and other shaped structures. Owing to the uniform fineness of the grain, the composition can be easily processed by the dry blend technique. Mixing of the components in the plasticized state is not required, To characterize the chlorinated low pressure polyethylenes to be used according to the invention the following methods were used: 1) Residue value according to the toluene/acetone (TAC) method: grams of the chloropolyethylene to be tested were re- ..H^ fluxed for 1 hour in 100 ml o a 1 : 1 mixture of toluene and acetone. The amount of insoluble residue consisting of insufficiently chlorinated portions is a measurement for the through chlorination of the polyethylene particles. The smaller the residue the better the chlorination product is suitable for the compositions of the invention. 2 ) Swelling value in methylcyclohexane (MCH) : The increase in weight of a sample after a 2h hour storage in methylcyclohexane is a further measurement for the through chlorination of the polyethylene particles.
Portions which have not been chlorinated to a sufficient extent swell very little. Products having a high swelling value are especially suitable.
The following examples illustrate the invention.
E X A M P L E 1 ; The chloropolyethylene used was prepared as follows: In a chlorination vessel 100 parts by weight of low pressure polyethylene having a reduced specific viscosity of 1 . 3 dl/g, in 900 parts by weight of 20 $ hydrochloric acid were chlorinated, first at 80°C until a chlorine content of 28 $ by weight had been reached and then at 121 . 5°C to a final chlorine content of 39. 2 by weight.
The product had a TAC value of 13 # and a MCH value of A mixture of 10 parts by weight of the above chlorination product and 90 parts by weight of suspension polyvinyl chloride having a K value of 70 was rolled for 10 minutes at 1 75°C with the addition of 3 parts by weight of barium/cadmium stabilize*^, and 1 part by weight of diphenyl-o ctyl phosphite. The plates moulded from the blend had the following values Notched impact strength according to DIN 53 > ¾53 M .7 cm g/cm 2 Impact strength at -20°C according to DIN 53 » ^53 "without break Notched tensile impact strength (DIN 53 , ¾¾8 ) 197 cmkg/cm2 COMPARATIVE EXAMPLE The same low pressure polyethylene was chlorinated under the conditions specified above, but in water without addition of hydrochloric acid. The polymer agglomerated to a large extent so that further chI>rination was much impeded. A chlorin-ation product was obtained having a chlorine content of 39. 1 by weight, a TAC value of ¾5 # and a MCH value of 3 $>» blend of 10 70 by weight of the said chlorination product with 0 by weight of suspension polyvinyl chloride having a K value of 70 , prepared under the conditions of Example 1 , was found to have a notched impact strength of 19.2 cmkg/cm and an impact strength at -20°C "without break" , according to DIN 53 » ^53 > and a notched tensile impact strength of 102 cmkg/cm according to DIN 53 , ^8.
E X A M P L E 2 : In a chlQrination vessel 1 00 parts by weight of low pressure polyethylene having a reduced specific viscosity of 1 . 2 dl/g in 1 200 parts by weight of 2h # hydrochloric acid to which 0. 48 part by weight of silicic acid having a mean particle size of 12 yum and an inner surface of 200 cm /g (BET) and 0.0¾8 part by weight of siloxane oil having a viscosity of 1 , 000 centi-stokes at 25°C had been added, were chlorinated, first at 80°C to a chlorine content of 20 # by weight, then the temperature was raised to 1 22 C and chlorination was continued until a chlorine content of 6. 6 $ by weight was reached. The product had a TAC value of 33 # and a MCH value of 16 A blend of 10 parts of the chloropolyethylene obtained with 90 parts of suspension PVC having a K value of 70 , prepared under the conditions specified in Example 1 , had a notched impact strength of 38 * 9 cmkg/cm and an impact strength at -20°C "without break" .
E X A M P L E 3_i \ In a chlorination vessel 1 00 parts by weight of low pressure polyethylene having a reduced specific viscosity of 3. 5 dl/g in 1 , 000 parts by weight of 20 by weight hydrochloric acid were chlorinated first at 70°C to a chlorine content of 20 by weight, then the temperature was raised to 126°C and chlorination was continued to a final chlorine content of 36. 3 $ by weight. The product obtained had a TAC value of 1 5 ^ and a MCH value of 21 A blend of 10 parts by weight of the chloropolyethylene with 90 parts by weight of suspension PVC having a K value of 70 , prepared according to claim 1 , had a notched impact strength of 51 . 3 cmkg/cm and an impact strength at -20 C "without break" .
Claims (8)
1. Thermoplastic composition essentially consisting of a) 98 to 50 by weight of a vinyl chloride polymer and b) 2 to 50 $ by weight of a chlorinated low pressure polyethylene having a chlorine content of 2 to hZ by weight, a reduced specific viscosity of 1 to dl/g, a residue value of 2 to kO measured by extraction in a 1 : 1 mixture of toluene and acetone, and a swelling value of 1 0 to 70 /¾, measured in methylcyclohexane , the chloro- poly-ethylene being prepared by chlorination of low pressure polyethylene in aqueous hydrochloric acid of 10 to 35 ^ strength by weight in the presence of 0 to 2 by weight of silicic acid and 0 to 1 . 0 by weight of siloxane oil, the percentages being calculated on the polyethylene, at a chlorination temperature of from °C to 1 30°C, at least 1 0 $ by weight of the chlorine being incorporated at a temperature of from 1 20 to 1 30°C.
2. . Thermoplastic composition as claimed in claim 1 , wherein the chloro-polyethylene used was prepared by chlorination starting at 50 to 1 00°C and ending at 1 20 to 1 30°C .
3. . Thermoplastic composition as claimed in claim 1 , wherein the chloro-polyethylene used was prepared by chlorination starting at 70 to 90°C and ending at 1 20 to 1 30°C. k. Thermoplastic composition as claimed in claim 1 , wherein the chlorinated low pressure polyethylene has a chlorine content of from 30 to ho
4. HOE 73/F 264
5. · " Thermoplastic composition as claimed in claim 1, wherein ^ the chlorinated polyethylene was prepared from low pressure polyethylene which had been thermally treated or pre- sintered at a temperature in the range of from 100°C to its crystallite melting point.
6. Process for the manufacture of a thermoplastic composition by mixing a) 8 to 50 70 by weight of a vinyl chloride polymer and b) 2 to 50 by weight of a chlorinated low pressure polyethylene wherein the said polyethylene has a chlorine content of 25 to 42 70 by weight, a reduced specific viscosity of 1 to 5 dl/g, a residue value of 2 to ho measured by extraction in a 1 : 1 mixture of toluene and acetone, and a swelling value of 10 to 70 measured in methylcyclo- hexane, and is prepared by chlorination in hydrochloric acid of 10 to 30 strength by weight in the presence of 0.1 to 2 70 by weight of silicic acid and 0.01 to 1.0 $ by weight of siloxane oil, the percentages being calculated on the polyethylene, at a chlorination temperature of from 50°C to 130°C, at least 10 # by weight of the chlorine being incorporated at a temperature of from 120 to 130°C.
7. · Process for the manufacture of the thermoplastic composition as claimed in claim 6, herein the viscosity number of the siloxane oil is in the range from 1000 to 500,000 centi stokes. HOE 73/F 26¾ '
8. Process for the manufacture of the thermoplastic composition as claimed in claim 6, wherein the quantity of silicic acid is from 0# 1 to 196 by weight. * Process for the manufacture of the thermoplastic composition as claimed in claim 6.wherein the silicic acid has an average particle size of from 1 to 50 H and an inner surface jof from 2 50 to kOO cm /g( according to BET). Attorneys for Applicant
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE2343982A DE2343982C3 (en) | 1973-08-31 | 1973-08-31 | Thermoplastic mass |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| IL45558A0 IL45558A0 (en) | 1974-11-29 |
| IL45558A true IL45558A (en) | 1977-06-30 |
Family
ID=5891279
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| IL45558A IL45558A (en) | 1973-08-31 | 1974-08-27 | Thermoplastic polivinylchloride composition |
Country Status (12)
| Country | Link |
|---|---|
| JP (1) | JPS5727912B2 (en) |
| AT (1) | AT329269B (en) |
| BE (1) | BE819448A (en) |
| CA (1) | CA1051580A (en) |
| CH (1) | CH598313A5 (en) |
| DE (1) | DE2343982C3 (en) |
| FR (1) | FR2242431B1 (en) |
| GB (1) | GB1475716A (en) |
| IL (1) | IL45558A (en) |
| IT (1) | IT1020309B (en) |
| NL (1) | NL7411333A (en) |
| SE (1) | SE394447B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS55110145A (en) * | 1979-02-14 | 1980-08-25 | Stauffer Chemical Co | Film forming composition |
| DE2914463A1 (en) * | 1979-04-10 | 1980-10-23 | Hoechst Ag | MEDICAL DEVICES FOR PARENTERAL LIQUIDS |
| DE2937178A1 (en) * | 1979-09-14 | 1981-04-02 | Hoechst Ag, 6000 Frankfurt | THERMOPLASTIC MASS |
| JPH042979Y2 (en) * | 1987-04-22 | 1992-01-31 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1275717A (en) * | 1970-02-09 | 1972-05-24 | Ici Ltd | Chlorination of polyethylene |
-
1973
- 1973-08-31 DE DE2343982A patent/DE2343982C3/en not_active Expired
-
1974
- 1974-08-15 CA CA207,124A patent/CA1051580A/en not_active Expired
- 1974-08-26 NL NL7411333A patent/NL7411333A/en not_active Application Discontinuation
- 1974-08-27 IL IL45558A patent/IL45558A/en unknown
- 1974-08-28 CH CH1174574A patent/CH598313A5/xx not_active IP Right Cessation
- 1974-08-29 IT IT26751/74A patent/IT1020309B/en active
- 1974-08-29 GB GB3786374A patent/GB1475716A/en not_active Expired
- 1974-08-30 AT AT705174A patent/AT329269B/en not_active IP Right Cessation
- 1974-08-30 SE SE7411022A patent/SE394447B/en unknown
- 1974-08-30 FR FR7429631A patent/FR2242431B1/fr not_active Expired
- 1974-08-30 JP JP9903874A patent/JPS5727912B2/ja not_active Expired
- 1974-09-02 BE BE148131A patent/BE819448A/en not_active IP Right Cessation
Also Published As
| Publication number | Publication date |
|---|---|
| GB1475716A (en) | 1977-06-01 |
| ATA705174A (en) | 1975-07-15 |
| IL45558A0 (en) | 1974-11-29 |
| DE2343982B2 (en) | 1978-12-07 |
| FR2242431A1 (en) | 1975-03-28 |
| BE819448A (en) | 1975-03-03 |
| SE7411022L (en) | 1975-03-03 |
| NL7411333A (en) | 1975-03-04 |
| SE394447B (en) | 1977-06-27 |
| JPS5727912B2 (en) | 1982-06-14 |
| JPS5064348A (en) | 1975-05-31 |
| DE2343982C3 (en) | 1979-08-09 |
| CH598313A5 (en) | 1978-04-28 |
| IT1020309B (en) | 1977-12-20 |
| FR2242431B1 (en) | 1978-02-17 |
| DE2343982A1 (en) | 1975-03-13 |
| CA1051580A (en) | 1979-03-27 |
| AT329269B (en) | 1976-05-10 |
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