GB1573174A - Process for preparing a compounding ingredient for vinyl chloride resins - Google Patents
Process for preparing a compounding ingredient for vinyl chloride resins Download PDFInfo
- Publication number
- GB1573174A GB1573174A GB1106777A GB1106777A GB1573174A GB 1573174 A GB1573174 A GB 1573174A GB 1106777 A GB1106777 A GB 1106777A GB 1106777 A GB1106777 A GB 1106777A GB 1573174 A GB1573174 A GB 1573174A
- Authority
- GB
- United Kingdom
- Prior art keywords
- tacky
- liquid
- powder
- vinyl chloride
- weight
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
-
- 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
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/203—Solid polymers with solid and/or liquid additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use 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; Derivatives of such polymers
- C08J2327/02—Characterised by the use 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; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/04—Characterised by the use 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; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08J2327/06—Homopolymers or copolymers of vinyl chloride
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Description
(54) PROCESS FOR PREPARING A COMPOUNDING
INGREDIENT FOR VINYL CHLORIDE RESINS
(71) We, SEKISUI KAGAKU KOGYO KABUSHIKI KAISHA, a
Japanese Company of No. 2, Kinugasa-cho, Kita-ku, Osaka-shi, Osaka, Japan, do hereby declare the invention for which we pray that a patent may be granted to us, and the method by which it is to be performed, to be particularly described in and by by the following statement:- This invention relates to a process for preparing a compounding ingredient for a vinyl chloride resin.
With conventional techniques, it is necessary to add a lubricant to a vinyl chloride resin for use in moulding to improve the workability of the resin during moulding and also it is necessary to add a stabilizer, such as an organotin stabilizer, to a vinyl chloride resin to be moulded to prevent heat deterioration of the resin. However, since conventionally used additives, such as a lubricant and an organotin stabilizer have a comparatively low melting point and such additives are mostly liquid or tacky at room temperature (e.g., 2e-30"C), such additives are difficult to use. More specifically, when a large amount of the additive is directly compounded in a vinyl chloride resin, it is difficult to disperse the additive uniformly in the resin simply using agitation because a localized adhesion of the resin occurs.This results in reducing the transportability of the product, hindering production, and decreasing the effects of stabilization of the resin.
In order to overcome the above described difficulty, a process has been proposed in which a liquid additive such as an organotin stabilizer is mixed with a part of the resin using a mixer having a strong shearing action to form a master powder and then the master powder is blended with the remainder of the resin in a ribbon blender as described in, for example, Plastic Zairyo Koza (Plastic Material Course), 14, Vinyl
Chloride Resins; pages 110--112, published by Nikkan Kogyo Shinbun Sha on October 15, 1961.
However, the above-described process has the disadvantage that, in producing a master powder in a granulated condition which is non-tacky and which can be easily handled, by compounding a liquid or a tacky compounding ingredient with a portion of an ordinary moulding suspension-polymerized vinyl chloride resin merely using the above-described process, only a master powder containing a very small proportion of the compounding ingredient can be obtained and thus the advantage of forming the master powder cannot sufficiently be utilized.
In compounding a liquid compounding ingredient with the resin, the ratio of the amount of resin to that of the liquid ingredient is at most 85/15 by weight. In compounding a tacky ingredient, the ratio-of the amount of resin to that of the tacky ingredient is at most 70/30 by weight.
A primary object of this invention is, therefore, to provide a process for preparing a compounding ingredient for vinyl chloride resins containing therein a high contact of an additive or additives such as a stabilizer, which is non-tacky, and which is granulated for handling convenience.
According to this invention, there is provided a process of preparing a granulated and non-tacky compounding ingredient for a vinyl chloride resin for moulding, comprising dry mixing (a) a liquid or tacky organotin stabilizer additive or a liquid or tacky organotin stabilizer additive and at least one other additive which may or may not be liquid or tacky with (b) a resin powder which is an emulsion-polymerized polyvinyl chloride or an emulsion-polymerized copolymer of vinyl chloride and another monomer copolymerizable therewith, said mixing being effected at a temperature of 100"C to llO"C and at a resin powder to liquid or tacky additive(s) weight ratio of 0.5-5:1.
The emulsion-polymerized polyvinyl chloride powder which is used in this invention is a so-called resin for paste and the particles of the resin powder are compact spheres having a smooth surface. The particle size of the resin powder is usually from 0.2 to 60 a. The weight ratio of the resin powder to the liquid or tacky additive(s) is preferably 1 to 2:1.
The average degree of polymerization (Pn) of the polyvinyl chloride preferably ranges from 900 to 1700, preferably from 1200 to 1400. The molecular weight (Mw) calculated based on the average degree of polymerization preferably ranges from 56250 to 106250, most preferably from 75000 to 87500.
The copolymers which may be used in this invention and are those usually used as resins for paste, for example, copolymers which are disclosed in Japanese Patent
Publication 2338/74 (column 7, lines 7 to 19), i.e., a copolymer of vinyl chloride and a monomer other than vinyl chloride which is copolymerizable with vinyl chloride, such as an olefin, e.g., ethylene, propylene or n-butene; a vinyl ester, e.g., vinyl acetate, vinyl propionate or vinyl laurate, vinyl stearate; an unsaturated acid and an ester thereof, e.g., acrylic acid, methacrylic acid or itaconic acid; a vinyl ether, e.g., methyl vinyl ether, ethyl vinyl ether, octyl vinyl ether or lauryl vinyl ether; maleic acid or maleic anhydride; fumaric acid or fumaric anhydride; an aromatic vinyl; an unsaturated carbonitrile; or a mixture thereof.
The amount of monomer capable of copolymerizing with vinyl chloride is prefer ably below 50% by weight based on the weight of the whole monomer composition.
A straight homopolymer of vinyl chloride is generally most preferred.
Examples of liquid or tacky organotin stabilizer additives include, as liquid additives, octyltin mercaptide, octyltin maleate, dibutyltin maleate, dioctyltin maleate, dibutyltin laurate, dibutyltin maleate laurate, dioctyltin laurate, dimethyltin carboxylic acid ester, dibutyltin mercapto carboxylic acid ester, dibutyltin sulfide, dioctyltin mercaptide and dioctyltin sulfide, and, as tacky additives, dibutyltin maleate polymer and dioctyltin maleate polymer. Examples of said at least one other additive include other stabilizers, such as certain kinds of metal soaps, for example, as liquid additives, calcium chlorostearate and barium chlorostearate, and as tacky additives, cadmium soap-epoxide; and hydrocarbon type lubricants, for example, as a liquid additives, liquid paraffin and, as tacky additives, polyethylene wax (low molecular weight polyethylene).
Examples of suitable mixers which can be used in compounding the additive(s) and the resin powder include a Henschel mixer and a supper mixer, with which mixing at high speed under heating can be achieved. The materials are mixed at 100 to 110 C. If the mixing is carried out at a temperature below about 100"C., a tacky powder is obtained and if the compounding is carried out at temperatures above about 1100C., a block product, which is not capable of practical use until it has been ground, is obtained.
Since the compounding ingredient prepared by the process of this invention can have a high additive(s) content, is non-tacky and is granulated (e.g. it may have a particle size distribution of 75 to 300 u), even when compounding it in a large amount of suspension-polymerized polyvinyl chloride usually employed in the art, the ingredient can be uniformly dispersed in the resin and hence no difficulties with respect to transportability as well as production occur.
The invention is explained in greater detail by reference to the following examples.
An emulsion-polymerized polyvinyl chloride having a mean polymerization degree of 1,300, a mean particle size of 50-60 microns, and an apparent specific gravity of 0.18 g./ml. and suspension-polymerized polyvinyl chloride having a mean polymerization degree of 800, a mean particle size of 170 microns, and an apparent specific gravity of 0.54 g./ml. were used in the examples.
Example 1.
To 55 parts by weight of an emulsion-polymerized polyvinyl chloride powder was compounded 45 parts by weight of liquid octyltin mercaptide using a Henschel mixer under heating employing the conditions as shown in Table 1. The results obtained are also shown in Table 1 below.
In addition, for the sake of comparison, to 55 parts by weight of a suspensionpolymerized polyvinyl chloride powder was compounded 45 parts by weight of liquid octyltin mercaptide under heating employing the same conditions as above and the results obtained are also shown in Table 1 below.
TABLE 1
*eu) u To, o oc u) *(l) *(2) *(3) *(l) *(2) *(3) E ~ ~ o . ~ ~ Compounding Su o , on Polymeri zed N Polyvinyl ('hioride r Mercaptide 45 45 45 45 45 45 (weight parts) ~ Rate (r.p m n. 1150 1150 1150 1150 1150 1150 o 7 ~ ~ t ~ Gv O Compounding Conditions Compounding Time 6 15 6.53 7.24 5.05 5.30 6.18 (min. sec.) H z ~ a C Grain Size 14.6 t 40.2.'59.8 66.133.9 o Tacky Tacky Tacky n ) Product lroduct Prduct w OIL vi Angle of Repose (0) 28 23 22 9 - = Specific 0.620 v) 0.702 - oo 0 Gravity s ~l ml) / E o 3 o g; s s ~ E E ~ S~l 6 .n / E e E c r n * In Table 1, 2 and 3, (1),(2) and (3) each represent samples produced from the same components, but under the different compounding conditions, especially compounding temperature, in Example 1 or in Comparison Example 1.
* Tacky product in Table 1 and 2, is not granulated because of tackiness.
As is clear from the results shown in Table 1 above, in Example 1, a desirable granulated product which was not tacky was obtained in each case, while in the comparison example, only a tacky block product was obtained in each case.
Example 2.
To 55 parts by weight of an emulsion-polymerized polyvinyl chloride powder were compounded 15 parts by weight of liquid octyltin mercaptide, 15 parts by weight of ocryltin maleate as a tacky powder, and 15 parts by weight of a liquid hydrocarbon lubricant (polyethylene wax of a molecular weight of 3000) using a Henschel mixer under heating employing the compounding conditions as shown in Table 2 below.
The results obtained are shown in Table 2 below.
In addition, for the sake of comparison, to 55 parts by weight of a suspensionpolymerized polyvinyl chloride powder were compounded the same additives as in the above example under heating employing the same compounding conditions as above and the results obtained are also shown in Table 2 below as Comparison Example 2.
Moreover, to 85 parts by weight of a suspension-polymerized polyvinyl chloride powder were compounded 5 parts by weight of liquid octyltin mercaptide, 5 parts by weight of octyltin maleate as a tacky powder, and 5 parts by weight of a liquid hydrocarbon lubricant under heating under the same compounding conditions as above and the results obtained are also shown in Table 2 below as Comparison Example 3. TABLE 2
& c Example 2 io ci = t1 *(2) 1n UE O (2) *(3) r 1 5^ r I c I 55 55 55 - - - - - ; ~. ~D X I , v, m v, parts) L,c oc - - 55 55 55 85 85 85 Polyvinyl Chloride (weigh parts) I -e " mCt Mercaptide 15 15 > D .,.
~ r i I m O vi Ir, I I 55 Maleate 15 15 r 15 15 15 5 5 5 Ê ~ c! m, m. ~ n n o o oo ~ X m '1 30 Rotation Rate (r.p.m.) 1150 > r l r l 1150 1150 1150 o cr s Ir. (C) m m o o r Q , oc ~ l rc,C O Condition Compounding Time (min. sec.) ------- 7.18 5.20 5.5 6.40 5.10 5.54 6 30 Cooling Time (min.) 15 15 15 15 15 15 15 15 15 ** Grain Size (250/250) 19.0.' 38.4 73.3/ Tacky Tacky Tacky 1.4.' 2.3 4.1 / 81.0 61.6 26.7 Product Pnduct Product 98.6 97.7 95.9 Pwduct Angle of Repose (0) 24 23 23 - - - 34 29 23 4 g Specific Gravity (g/ml) 0.634 0.712 0.748 - - - 0.638 .O, 0.662 As is clear from the results shown in Table 2 above, when 45 parts by weight of the liquid and tacky additives were compounded with 55 parts by weight of the emulsion-polymerized polyvinyl chloride powder under the compounding temperature conditions of l00-1100C. as in Example 1, a desirable granulated product which was not tacky was obtained in each case. On the other hand, when the same additives as in Example 2 were compounded with 55 parts by weight of suspension-polymerized polyvinyl chloride under the same conditions as above as in Comparison Example 2, only a tacky block product was obtained in each case.When a comparatively small amount, i.e., 15 parts by weight of the same liquid and tacky additives were compounded with 85 parts by weight of suspension-polymerized polyvinyl chloride under the same conditions as above in Comparison Example 3, a granular non-tacky product was obtained in each case but the granular condition of the products was poor and the products were all inconveniertt to handle.
As described above, by compounding liquid and tacky additives with the emulsion polymerized polyvinyl chloride powder under heating at 100--1100C. according to this invention desirable granulated compounding ingredients having a high additive content and which are non-tacky can be obtained.
Examples 3 and 4.
To 35 parts by weight of an emulsion-polymerized polyvinyl chloride powder were compounded 10 parts by weight of liquid octyltin mercaptide, 10 parts by weight of octyltin maleate as a tacky powder, 10 parts by weight of a liquid hydrocarbon lubricant (polyethylene wax of a molecular weight of 3000), and 35 parts by weight of calcium carbonate powder using a Henschel mixer under heating employing the compounding conditions as shown in Table 3 below. Furthermore, to 30 parts by weight of an emulsion-polymerized polyvinyl chloride powder were compounded 15 parts by weight of liquid octyltin mercaptide, 15 parts by weight of octyltin maleate as a tacky powder, 15 parts by weight of a liquid hydrocarbon lubricant (polyethylene wax of a molecular weight of 3000), and 25 parts by weight of a silicic acid powder under the same conditions as above. The results obtained are shown in Table 3 below.
TABLE 3
Example 3 Example 4 *(l) *(2) *(3) * (1) * (2) * (3) " 35 35 35 30 30 30 cl Chloride (weight parts) Octyltin Mercaptide 10 10 10 15 15 IS 9 parts) V ? X Components (weight parts) < Carbonate ç 35 I 35 9 ,c. l O -- rl Silicic Acid (weight parts) - - - 25 25 25 Rotation Rate (r.p.m.) 1150 1150 1150 1150 1150 1150 WX Temperature (0C) 100 105 110 100 105 110 m 3 Compounding Time (min. sec.) 5.20 6.03 6.47 6.08 6.53 7.40 vr Time (min.) 15 15 15 15 15 15 A X Product 73.7 47.9 '" Angle of Repose (0) d 23 24 24 23 23 a Specific Gravity > > 0.782 0.843 0.608 0.654 0.676 A | E E D D ffi As is clear from the results shown in Table 3 above, when a powdery filler such as calcium carbonate powder and silicic acid powder was compounded with the emulsion-polymerized polyvinyl chloride powder together with other, liquid and tacky, additives according to the process of this invention, desirable granulated compounding ingredients having a high additive content such as the above-described liquid and tacky stabilizers and lubricant, and which are non-tacky can be obtained.
WHAT WE CLAIM IS: 1. A process of preparing a granulated and non-tacky compounding ingredient for a vinyl chloride resin for moulding, comprising dry mixing (a) a liquid or tacky organotin stabilizer additive or a liquid or tacky organotin stabilizer additive and at least one other additive which may or may not be liquid or tacky with (b) a resin powder which is an emulsion-polymerized polyvinyl chloride or an emulsion-polymerized copolymer of vinyl chloride and another monomer copolymerizable therewith, said mixing being effected at a temperature of 100"C to 1100C and at a resin powder to liquid or tacky additive(s) weight ratio of 0.5-5:1.
2. A process as claimed in claim 1, wherein said resin powder is an emulsionpolymerized polyvinyl chloride.
3. A process as claimed in claim 1, wherein said resin powder is an emulsionpolymerized copolymer of vinyl chloride and another monomer copolymerizable therewith.
4. A process as claimed in claim 3, wherein the copolymer is formed from a monomer composiUon containing less than 50% by weight of said another monomer.
5. A process as claimed in any preceding claim, wherein said weight ratio is 1 6. A process as claimed in any preceding claim, wherein said organotin stabilizer is octyltin mercatide or octyltin maleate.
7. A process as claimed in claim 1, substantially as hereinbefore described in any one of Examples 1 to 4.
8. A granulated and non-tacky compounding ingredient for a vinyl chloride resin when prepared by the process as claimed in any preceding claim.
**WARNING** end of DESC field may overlap start of CLMS **.
Claims (8)
1. A process of preparing a granulated and non-tacky compounding ingredient for a vinyl chloride resin for moulding, comprising dry mixing (a) a liquid or tacky organotin stabilizer additive or a liquid or tacky organotin stabilizer additive and at least one other additive which may or may not be liquid or tacky with (b) a resin powder which is an emulsion-polymerized polyvinyl chloride or an emulsion-polymerized copolymer of vinyl chloride and another monomer copolymerizable therewith, said mixing being effected at a temperature of 100"C to 1100C and at a resin powder to liquid or tacky additive(s) weight ratio of 0.5-5:1.
2. A process as claimed in claim 1, wherein said resin powder is an emulsionpolymerized polyvinyl chloride.
3. A process as claimed in claim 1, wherein said resin powder is an emulsionpolymerized copolymer of vinyl chloride and another monomer copolymerizable therewith.
4. A process as claimed in claim 3, wherein the copolymer is formed from a monomer composiUon containing less than 50% by weight of said another monomer.
5. A process as claimed in any preceding claim, wherein said weight ratio is 1
6. A process as claimed in any preceding claim, wherein said organotin stabilizer is octyltin mercatide or octyltin maleate.
7. A process as claimed in claim 1, substantially as hereinbefore described in any one of Examples 1 to 4.
8. A granulated and non-tacky compounding ingredient for a vinyl chloride resin when prepared by the process as claimed in any preceding claim.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2968176A JPS52111953A (en) | 1976-03-17 | 1976-03-17 | Preparation of compounding additives for vinyl chloride resins |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| GB1573174A true GB1573174A (en) | 1980-08-20 |
Family
ID=12282848
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB1106777A Expired GB1573174A (en) | 1976-03-17 | 1977-03-16 | Process for preparing a compounding ingredient for vinyl chloride resins |
Country Status (9)
| Country | Link |
|---|---|
| JP (1) | JPS52111953A (en) |
| AU (1) | AU504155B2 (en) |
| CA (1) | CA1102461A (en) |
| DE (1) | DE2711775C3 (en) |
| ES (1) | ES456962A1 (en) |
| FR (1) | FR2344592A1 (en) |
| GB (1) | GB1573174A (en) |
| IT (1) | IT1083734B (en) |
| NL (1) | NL165199C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60500247A (en) * | 1982-02-01 | 1985-02-28 | ブス アクチエンゲゼルシヤフト | Method and apparatus for continuous production of flowable homogeneous mixture of plastic and additives |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NL224073A (en) * | 1957-01-18 | |||
| US3301813A (en) * | 1963-03-22 | 1967-01-31 | Monsanto Co | Process for incorporating a liquid additive into a solid thermoplastic polymer |
| FR1429010A (en) * | 1964-03-30 | 1966-02-18 | Knapsack Ag | Process for the preparation of mixtures based on vinyl resins containing adjuvants |
| BE769094A (en) * | 1970-07-06 | 1971-11-03 | Reagens Spa | PROCESS FOR PACKAGING ADDITIVES AND ADDITIVES CONDITIONED BY THE PROCESS |
-
1976
- 1976-03-17 JP JP2968176A patent/JPS52111953A/en active Pending
-
1977
- 1977-03-14 CA CA273,912A patent/CA1102461A/en not_active Expired
- 1977-03-15 IT IT4847277A patent/IT1083734B/en active
- 1977-03-16 AU AU23300/77A patent/AU504155B2/en not_active Expired
- 1977-03-16 GB GB1106777A patent/GB1573174A/en not_active Expired
- 1977-03-17 FR FR7708043A patent/FR2344592A1/en active Granted
- 1977-03-17 ES ES456962A patent/ES456962A1/en not_active Expired
- 1977-03-17 DE DE19772711775 patent/DE2711775C3/en not_active Expired
- 1977-03-17 NL NL7702899A patent/NL165199C/en not_active IP Right Cessation
Also Published As
| Publication number | Publication date |
|---|---|
| CA1102461A (en) | 1981-06-02 |
| FR2344592B1 (en) | 1981-09-11 |
| JPS52111953A (en) | 1977-09-20 |
| NL165199C (en) | 1981-03-16 |
| AU504155B2 (en) | 1979-10-04 |
| AU2330077A (en) | 1978-09-21 |
| IT1083734B (en) | 1985-05-25 |
| DE2711775B2 (en) | 1980-03-06 |
| NL7702899A (en) | 1977-09-20 |
| ES456962A1 (en) | 1978-01-16 |
| DE2711775C3 (en) | 1986-01-09 |
| NL165199B (en) | 1980-10-15 |
| FR2344592A1 (en) | 1977-10-14 |
| DE2711775A1 (en) | 1977-09-22 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PS | Patent sealed | ||
| PCNP | Patent ceased through non-payment of renewal fee |