CN115725117A - Antioxidant dispersion liquid, preparation method thereof, terminator composition containing antioxidant dispersion liquid and application thereof - Google Patents
Antioxidant dispersion liquid, preparation method thereof, terminator composition containing antioxidant dispersion liquid and application thereof Download PDFInfo
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Abstract
Antioxidant dispersion liquid, a preparation method thereof, a terminator composition containing the antioxidant dispersion liquid and application thereof. The invention relates to an antioxidant dispersion liquid, a preparation method thereof, a terminator composition containing the antioxidant dispersion liquid and application thereof, belonging to the technical field of suspension method vinyl chloride polymerization. The antioxidant dispersion liquid of the present invention comprises: 1-40 parts of thioester antioxidant, 0-30 parts of phenol antioxidant, 0.01-4 parts of alkylphenol polyoxyethylene ether emulsifier, 0.05-1.0 part of water-soluble polymer stabilizer and 55.0-99.0 parts of pure desalted water. The invention provides an antioxidant dispersion liquid for improving the thermal stability of PVC, provides a simple and convenient preparation method of the antioxidant dispersion liquid, and also provides a terminator composition containing the antioxidant dispersion liquid, which reduces introduction of chemical substances which are unfavorable to post-treatment and processing and manufacturing molding processes into PVC resin products as much as possible on the basis of ensuring the termination efficiency and effect of vinyl chloride polymerization, and reduces the adverse effects of foreign substances on the performance of the resin and the finished products.
Description
Technical Field
The invention relates to an antioxidant dispersion liquid, a preparation method thereof, a terminator composition containing the antioxidant dispersion liquid and application thereof, and belongs to the technical field of suspension method vinyl chloride polymerization.
Background
Polyvinyl chloride (PVC) resin has the excellent characteristics of flame retardancy, chemical corrosion resistance, wear resistance, low cost, easiness in molding and processing and the like, but has poor thermal stability. In the suspension polymerization production process widely adopted in the field of PVC resin manufacturing, the subsequent process and the resin processing and using process are usually subjected to operation treatment such as heating, and the protection of the PVC resin is very important.
As an assistant for improving the suspension PVC resin product, terminators such as ASTC (Acetonthiosemicarbazone), bisphenol A (4, 4' -dihydroxydiphenylpropane) and DEHA (diethylhydroxylamine) are still widely used in production. These adjuvants have either a potential risk in terms of biochemical toxicity or are still insufficient in terms of the effect of improving thermal stability.
In order to improve the thermal stability of PVC resin products, a combined application method of diethylhydroxylamine with pentaerythritol tetrakis (3-laurylthiopropionate) and octadecyl-3- (3, 5-di-t-butyl-4-hydroxyphenyl) propionate is provided in the document of application No. 201810823048.0, and an antioxidant is subjected to a shear emulsification operation under heating. In the method, the stirring mechanical strength is obviously insufficient, the antioxidant particles dispersed under the heating condition are cooled to normal temperature without sufficient protection, particle coalescence can be generated in the cooling process, and more importantly, a sulfur-containing group emulsifier with strong low-molecular adsorbability is used, so that the performances of the apparent density, the plasticizer absorption and the like of the PVC resin can be influenced.
CN109879995 describes a terminator for vinyl chloride polymerization, which is composed of surfactant, polymerization inhibitor, antioxidant, thickener and water, wherein the surfactant is alkylphenol ethoxylates, fatty alcohol polyoxyethylene ether sulfate, higher alcohol, etc., the polymerization inhibitor is nitroxide free radical compound, the antioxidant is at least one of hindered phenol antioxidant, thioester antioxidant or phosphite antioxidant, and the thickener is gum or polyvinyl alcohol. According to the technical scheme provided by the document, the nitroxide free radical compound is used as a terminator and is used together with an antioxidant in a preparation process, so that the terminating effect and the heat-resistant modification effect cannot be fully considered, and the use cost is increased. In addition, the technical scheme of the document provides a plurality of antioxidant using methods, not only the influence of the density difference between the antioxidant and water on the stability of the dispersion liquid is not noticed, the unnecessary using amount of the emulsifier or the thickener is increased, but also the synergistic effect between the phenolic antioxidant and the thioester antioxidant is not considered.
Patent document CN107474167 provides a vinyl chloride polymerization termination method which adds a conventional terminator and a thioester type antioxidant after completion of vinyl chloride polymerization, allows rapid termination of polymerization and improves the aged whiteness of the resulting polyvinyl chloride product. However, the technical scheme of the document is lack of the influence of the density of the antioxidant on the stability of the emulsion, the standing stability of the emulsion is still not fully solved, the synergistic effect of the thioester antioxidant and the phenol antioxidant is not exerted, and the thermal stability improvement effect is still insufficient.
Disclosure of Invention
The invention aims to provide an antioxidant dispersion liquid for improving the thermal stability of PVC, provides a simple and convenient preparation method of the antioxidant dispersion liquid, and also provides a terminator composition containing the antioxidant dispersion liquid, which reduces introduction of chemical substances which are unfavorable to post-treatment and processing and manufacturing molding processes into PVC resin products as much as possible on the basis of ensuring the termination efficiency and effect of vinyl chloride polymerization, and reduces the adverse effect of foreign substances on the performance of the resin and the finished product.
The antioxidant dispersion liquid provided by the invention comprises the following raw materials in parts by weight:
preferably, the thioester antioxidant is DLTDP (dilauryl thiodipropionate), DTDTDTP (ditridecyl thiodipropionate), DMTDP (ditetradecyl thiodipropionate) or DSTDP (distearyl thiodipropionate).
The phenolic antioxidant is a low-molecular monophenol antioxidant. BHT (2, 6-di-tert-butyl-p-cresol), BBHT (2, 6-bis (. Alpha. -methyl-phenyl) -4-methylphenol) or SP (styrenated benzene powder) are preferred.
Preferably, the alkylphenol polyoxyethylene ether emulsifier is OP-7, OP-9, OP-10 or OP-13 having an HLB (hydrophilic lipophilic balance) of 10 to 14.
Preferably, the water-soluble polymeric stabilizer is polyvinyl alcohol having an average molecular weight of 75-95% alcoholysis and a Brookfield viscosity of 28-70 mPs in a 4% aqueous solution. Further preferred are KH-17, KH-20, FS-20, 35-80, 48-80 and FS-22H.
The preparation method of the antioxidant dispersion liquid comprises the following steps:
mixing thioester antioxidant, phenol antioxidant, alkylphenol polyoxyethylene ether emulsifier and part of desalted water, heating to 40-95 deg.C, shearing, emulsifying, dispersing, cooling to room temperature, adding water soluble polymer stabilizer and the rest desalted water, and making into antioxidant dispersion liquid with average particle size less than 5.0 μm.
A terminator composition comprises the above antioxidant dispersion liquid and hydroxylamine terminators.
Preferably, the hydroxylamine based terminator is Diethylhydroxylamine (DEHA) or N-Isopropylhydroxylamine (IPHA).
Preferably, the hydroxylamine-based terminator is used in an amount of 0.01 to 0.20% by mass based on the vinyl chloride monomer.
Preferably, the antioxidant dispersion is used in an amount of 0.02 to 0.5%.
The terminator composition is used for suspension method vinyl chloride polymerization.
The results of past studies have demonstrated that the thermal stability of PVC resins, one of the widest range of applications, is always the most interesting property in use. The PVC resin can generate a reaction of removing hydrogen chloride molecules under the heated condition, and the hydrogen chloride has the function of accelerating the decomposition of the PVC resin. If peroxide initiators remain in the PVC polymer, or in the presence of oxygen, products containing hydrogen peroxide are also generated during the thermal decomposition of the heated PVC resin. The presence of both peroxides generates free radicals, which accelerate the thermal decomposition of the PVC resin. In terms of improving thermal stability, thioester antioxidants have unique advantages, and have unique decomposition and peroxide elimination effects. The research of the invention proves that after the PVC resin obtained by polymerization is added with the thioester antioxidant, the thermal stability of the resin is greatly improved especially under the standard test conditions (160 ℃,10 min).
Thioester antioxidants are often used in the form of an emulsified dispersion. However, metering deviation and using effect of thioester antioxidants are easily caused when the dispersion is not uniformly prepared, so that the stability of the dispersion has an important influence on the improvement of the thermal stability of the PVC resin. The research of the invention finds that under the condition of referring to the density of the thioester antioxidant, the thioester antioxidant or the compound thereof is ensuredHas a density difference of less than 0.05g/cm with respect to the water as the dispersion medium 3 In this case, an appropriate amount of an alkylphenol polyoxyethylene ether emulsifier having a certain performance and a water-soluble polymer stabilizer are added to obtain an antioxidant dispersion liquid having excellent stability.
In the invention, the phenolic antioxidant is used as an antioxidant which can be used for compounding, has the main functions of providing density adjustment, and can generate synergistic action with the thioester antioxidant to further enhance the thermal stability of the antioxidant.
The thioester antioxidant exists mainly in solid powder state (except DTDTP) at normal temperature, and the average particle diameter of the finished product particles is usually more than 20 μm. Although the difference between the density of the compound or the compound and the monophenolic antioxidant and the medium water can be less than 0.05g/cm 3 However, if the average particle size of the particles is larger than 5 μm and the surfactant is not properly and sufficiently present, the stability of the antioxidant dispersion is not ensured.
In order to ensure that the average particle size of the thioester antioxidant or a compound of the thioester antioxidant and the monophenol antioxidant is less than 5 μm, various processes can be selected, the used equipment can include, but is not limited to, a high-speed shearing machine, a colloid mill, a tubular homogenizer and the like, and particularly, the dispersing and emulsifying mode is not limited. The antioxidant is crushed and emulsified by a shearing emulsifying machine and the like to obtain the antioxidant with the arithmetic mean particle size of less than 5 mu m, thereby providing basic conditions for improving the stability of the antioxidant dispersion.
For better pulverization and emulsification, it is preferable to carry out the pulverization and emulsification in a liquid state in which the viscosity of the antioxidant is low, and in this case, the treatment temperature should preferably be higher than the melting point of the antioxidant (usually at atmospheric pressure). In the present invention, the heat treatment temperature is in the range of from the melting point of the antioxidant to 100 ℃ and preferably from 40 to 95 ℃. In actual operation, the temperature is selected depending on the melting point of the antioxidant, namely, because the liquid antioxidant has low hardness and small viscosity, the optimal dispersion effect can be obtained by carrying out high-strength shearing treatment on the antioxidant in a liquid state, and the treatment time is relatively short, so that the production efficiency is favorably improved.
During the crushing and emulsifying process, a proper emulsifier should be selected to disperse and protect the antioxidant particles. Alkylphenol polyoxyethylene ethers are found to be suitable emulsifiers in the present invention, and OP-7, OP-9, OP-10 and OP-13 having HLB values (hydrophilic lipophilic balance) of 10 to 14 are preferred in the present invention. Under the condition, the average particle size of the thioester antioxidant or the compound particle thereof can be below 5 mu m, and the thioester antioxidant or the compound particle thereof can keep good stability during storage.
Although the average particle size of the antioxidant dispersion liquid subjected to mechanical dispersion and emulsification can be lower than 5 micrometers, the problems that the antioxidant particles are distributed with a certain width, large particles exist in the dispersion liquid, and the large particles can agglomerate and further settle and separate out due to adsorption are considered.
By the above treatment process, an antioxidant dispersion having an average particle size of 5 μm at room temperature and good standing stability can be obtained.
The antioxidant dispersion has a large effect of improving the thermal stability of PVC resin, but does not have a rapid termination effect on the suspension polymerization of vinyl chloride. In addition, in order to achieve the rapid termination effect, the amount of the antioxidant needs to be greatly increased, so that the use cost of the antioxidant is increased, and the economy is poor. In order to improve the termination effect on vinyl chloride, a conventional terminator such as bisphenol A, ATSC (acetonic thiosemicarbazone), DEHA (diethylhydroxylamine) or the like may be added to the above antioxidant dispersion. In the present invention, low-toxic DEHA (diethylhydroxylamine) and IPHA (N-isopropylhydroxylamine) are preferably used in an amount of 0.05 to 0.20% (50 to 2000 ppm) based on the mass of vinyl chloride monomer.
The invention applies the composition consisting of the antioxidant dispersion liquid and the terminator to the vinyl chloride monomer homopolymerization polymerization process adopting the suspension method.
For the suspension polymerization of vinyl chloride to which the present invention is applicable, the reaction temperature is in the range of 45 to 70 ℃, and is particularly effective for reaction systems using peroxide initiators. Initiators commonly used in suspension polymerization include dialkyl peroxydicarbonates, such as EHP (bis (2-ethylhexyl) peroxydicarbonate); alkyl peroxides such as TBPND (t-butyl peroxyneodecanoate), ACPND (cumyl peroxyneodecanoate), and the like; dialkyl acyl peroxides, such as dilauroyl peroxide, and the like; azobiscyanolides such as azobisisoheptonitrile and the like. The amount of initiator is determined according to the reaction temperature and the time required in the process, and is generally 0.02 to 0.20% by mass of the vinyl chloride monomer.
The vinyl chloride suspension polymerization system to which the present invention is applied is not limited, and the dispersing agent for polymerization is mainly a polyvinyl alcohol or a dispersing agent system formed by compounding with methyl cellulose. Similarly, a vinyl chloride polymerization auxiliary dispersant other than the primary dispersant may be used, such as a low alcoholysis degree polyvinyl alcohol, sorbitan fatty acid ester, and the like, and the present invention is not limited thereto. Other conditions of suspension polymerization of vinyl chloride, such as water-oil ratio, stirring speed, feeding mode, and other polymerization aids such as molecular weight regulator, pH regulator, etc., are not limited in the present invention, and can be used without significantly affecting the present invention.
Compared with the prior art, the invention has the following beneficial effects:
(1) The antioxidant dispersion liquid prepared by the invention has good standing stability and can be used for improving the thermal stability of PVC;
(2) The invention provides a simple and convenient preparation method of the antioxidant dispersion liquid, and limits the average granularity range of the antioxidant dispersion liquid;
(3) When the prepared antioxidant dispersion liquid is mixed with the selected terminator and then used for vinyl chloride polymerization by a suspension method, on the basis of ensuring the termination efficiency and effect of vinyl chloride polymerization, chemical substances which are unfavorable to post-treatment and processing manufacturing molding processes are introduced into PVC resin products to the greatest extent, and the adverse effects of foreign substances on the performance of the resin and finished products are reduced.
Detailed Description
The present invention will be described in detail below with reference to specific examples, but the present invention is not limited to these examples.
The analysis method comprises the following steps:
1. the stability analysis method of the antioxidant dispersion liquid comprises the following steps:
the prepared antioxidant emulsion dispersion was placed in a closed 500mL colorless wide-necked glass bottle, and the solution was allowed to stand in the shade for 7 days (7 days × 24 hours) and then observed.
2. Vinyl chloride resin thermal stability test method:
the method is carried out according to the GB/T15595-1995 standard determination method, and the test conditions are as follows: 160 ℃ for 10min.
Example 1
30 parts of antioxidant DSTDP, 30 parts of desalted water and 3 parts of emulsifier OP-10 are taken, heated to 70 ℃, dispersed for 10min at 20000rpm by a Frouk FA25 shearing emulsifying machine, then 36.5 parts of desalted water is added, cooled to normal temperature, and then 0.5 part of polyvinyl alcohol dispersant KH-20 (product of Japan synthetic chemical company, average polymerization degree 2000, alcoholysis degree 81.0%, brookfield rotary viscosity of 4% water solution 49.1 mPa.s) is added to prepare antioxidant DSTDP dispersion liquid with the content of about 30%, and the density of the antioxidant is about 1.03g/mL at normal temperature.
The antioxidant emulsion arithmetic mean particle size is measured by a Mastersizer2000 laser particle size analyzer to be 2.7 mu m. After 7 days, the emulsion was observed, and the number average particle size of the antioxidant emulsion was measured again to be 3.4. Mu.m, without causing any delamination.
2400 parts of desalted water, 0.20 part of polyvinyl alcohol KH-20 (Japanese synthetic chemical product), 0.25 part of hydroxypropyl methylcellulose E50 (American chemical product), 0.2 part of polyvinyl alcohol LW-200 (dispersion aid, japanese synthetic chemical product), 0.2 part of TAPP (pivaloyl peroxypivalate), and 0.20 part of TBPND (t-butyl peroxyneodecanoate) were charged into a stainless steel autoclave equipped with a stirrer. And (3) replacing the air in the kettle, vacuumizing, adding 1500 parts of vinyl chloride, starting stirring, and heating to 63.5 ℃ for reaction. After the pressure is reduced by 0.20MPa, a terminator mixed solution which is composed of 0.25 part of DEHA (diethylhydroxylamine) and 2.0 parts of DSTDP antioxidant emulsion is added into the kettle. Removing unreacted vinyl chloride monomer in the reaction kettle, dehydrating the obtained slurry to obtain wet material, and drying at 60 ℃ for 6 hours to obtain PVC resin dry powder.
The ageing whiteness of the resin is measured by the GB/T15595-1995 test method of the obtained resin dry powder, and the obtained results are listed in Table 1.
Example 2
Taking 15 parts of antioxidant DLTDP, 18.8 parts of antioxidant BHT, 35 parts of desalted water and 4 parts of emulsifier OP-10, heating to 75 ℃, dispersing for 10min at 25000rpm by using a Frouk FA25 shearing emulsifying machine, then adding 26.4 parts of desalted water, cooling to normal temperature, then adding 0.8 part of polyvinyl alcohol KH-17 (a product of Japan synthetic chemical company, with the average polymerization degree of 1700, the alcoholysis degree of 81.0 percent and the Brookfield rotary viscosity of 4 percent of water solution of 34.5 mPa-s) to prepare the antioxidant DLTDP/BHT dispersion liquid with the content of about 33.8 percent, wherein the density of the composite antioxidant is about 0.97g/mL at normal temperature.
The antioxidant emulsion arithmetic mean particle size is measured by a Mastersizer2000 laser particle size analyzer to be 2.6 mu m. And (4) standing for 7 days, observing the condition of the emulsion, wherein no layering phenomenon exists, and determining the arithmetic mean particle size of the antioxidant emulsion to be 3.1 mu m.
The vinyl chloride reaction formulation and process of example 1 were used for evaluation tests. Except that 0.25 parts DEHA and 1.78 parts DLTDP/BHT dispersion were used.
After the obtained resin slurry is centrifugally dewatered and dried, the aging whiteness of the resin is measured by a GB/T15595-1995 test method, and the obtained results are shown in Table 1.
Example 3
Taking 10 parts of antioxidant DTDTP, 8.2 parts of antioxidant SP, 30 parts of desalted water and 0.1 part of emulsifier OP-13, heating to 40 ℃, dispersing for 10min at 15000rpm by using a Frouk FA25 shearing emulsifying machine, then adding 51.5 parts of desalted water, cooling to normal temperature, and then adding 0.2 part of polyvinyl alcohol FS-20 (medium and petrochemical vinyl chemical products, average polymerization degree 1957, alcoholysis degree 80.6%, brookfield rotary viscosity of 4% aqueous solution 47.8mPa & s) to prepare antioxidant DTDTP/SP dispersion with the content of about 18.2%, wherein the density of the composite antioxidant is about 1.00g/mL at normal temperature.
The antioxidant emulsion arithmetic mean particle size was 4.4 μm measured using a Mastersizer2000 laser particle sizer. And (3) standing for 7 days, observing the condition of the emulsion, wherein no layering phenomenon exists, and determining the arithmetic mean particle size of the antioxidant emulsion to be 4.8 mu m.
The vinyl chloride reaction formulation and process of example 1 were used for evaluation tests. Except that 0.35 parts of IPHA and 2.88 parts of DTDTP/SP dispersion were used.
After the obtained resin slurry is subjected to centrifugal dehydration and drying, the aging whiteness of the resin is measured by a test method of GB/T15595-1995, and the obtained results are listed in Table 1.
Example 4
Taking 5 parts of antioxidant DMDTP, 6.5 parts of antioxidant BBHT, 20 parts of desalted water and 0.6 part of emulsifier OP-9, heating to 55 ℃, dispersing for 10min at 20000rpm by using a Fracuk FA25 shearing emulsifying machine, then adding 67.8 parts of desalted water, cooling to normal temperature, adding 0.2 part of polyvinyl alcohol FS-22H (medium and petrochemical vinyl chemical products, alcoholysis degree of 88.4%, brookfield rotary viscosity of 4% aqueous solution of 47.4mPa s), and preparing antioxidant DMDTP/BBHT dispersion liquid with the content of about 11.5%, wherein the density of the composite antioxidant is about 0.99g/mL at normal temperature.
The antioxidant emulsion has a calculated average particle size of 4.8 μm as determined by a Mastersizer2000 laser particle size analyzer. And (3) standing for 7 days, observing the condition of the emulsion, wherein no layering phenomenon exists, and determining the arithmetic mean particle size of the antioxidant emulsion to be 5.0 mu m.
The vinyl chloride reaction formulation and process of example 1 were used for evaluation tests.
Except that 0.15 parts DEHA and 5.87 parts DMDTP/BBHT dispersion were used. After the obtained resin slurry is centrifugally dewatered and dried, the aging whiteness of the resin is measured by a GB/T15595-1995 test method, and the obtained results are shown in Table 1.
Comparative example 1
An antioxidant dispersion liquid is prepared by taking 15 parts of an antioxidant DLTDP, 18.8 parts of an antioxidant BHT, 35 parts of desalted water and 4 parts of an emulsifier OP-10 in example 2, the difference is that after the antioxidant DLTDP is heated to 75 ℃, a common reinforced stirrer is adopted to disperse and stir at 2300rpm for about 11 minutes, after the antioxidant DLTDP is cooled to normal temperature, 26.4 parts of desalted water and 0.8 part of polyvinyl alcohol KH-17 are added, the arithmetic mean particle size of the antioxidant dispersion liquid is measured to be about 147 mu m, after the antioxidant DLTDP is kept stand for 20 hours, the antioxidant is layered, namely, the antioxidant is precipitated due to particle coalescence, and at the moment, when the particle size of the antioxidant DLTDP is measured again, a stable test result cannot be obtained due to large fluctuation of results.
Comparative example 2
The antioxidant formula and preparation method of example 2 are adopted, except that a Fruke FA25 shearing emulsifying machine disperses for 2 minutes at 10000rpm, the density of the composite antioxidant is 0.97g/mL at normal temperature, the arithmetic mean particle size of antioxidant particles of the dispersion is 7.7 μm, and the dispersion is layered after standing for 48 hours at normal temperature.
Comparative example 3
The antioxidant formulation and formulation of example 2 were used except that 0.8 part of polyvinyl alcohol KH-17 was not used, and at this time the dispersion had an average particle size of 3.6 μm, but the dispersion was allowed to stand at room temperature for 48 hours before demixing occurred.
Comparative example 4
The antioxidant formulation and preparation method of example 2 were used, except that emulsifier OP-10 was replaced with emulsifier OP-3 (HLB value about 4-5), the resulting normal temperature antioxidant dispersion had a arithmetic mean particle size of 6.4 μm, and the dispersion was allowed to stand at room temperature for 48 hours and then delaminated.
Comparative example 5
The vinyl chloride polymerization formulation and operating process conditions of example 1 were employed. The composite antioxidant dispersion liquid is not used when the reaction is terminated, and 0.25 part of DEHA is used as the terminator.
After the resulting resin slurry was dried, the aged whiteness of the resin was measured by the test method of GB/T15595-1995, and the results are shown in Table 1.
TABLE 1 antioxidant Dispersion stability and Heat stability test results for terminated reaction products
Claims (10)
1. An antioxidant dispersion liquid, characterized in that: the composite material comprises the following raw materials in parts by mass:
2. the antioxidant dispersion liquid according to claim 1, wherein: the thioester antioxidant is dilauryl thiodipropionate, ditridecyl thiodipropionate, ditetradecyl thiodipropionate or distearyl thiodipropionate.
3. The antioxidant dispersion liquid according to claim 1, wherein: the phenol antioxidant is 2, 6-di-tert-butyl-p-cresol, 2, 6-di (alpha-methyl-phenyl) -4-methylphenol or styrenated benzene powder.
4. The antioxidant dispersion liquid according to claim 1, wherein: the alkylphenol polyoxyethylene ether emulsifier is OP-7, OP-9, OP-10 or OP-13 with the hydrophile-lipophile balance value of 10-14.
5. The antioxidant dispersion liquid according to claim 1, wherein: the water-soluble high molecular stabilizer is polyvinyl alcohol with average molecular weight of 75-95% alcoholysis degree and Brookfield viscosity of 28-70 mP.s in 4% water solution.
6. A method for producing the antioxidant dispersion liquid according to any one of claims 1 to 5, characterized in that: the method comprises the following steps:
mixing thioester antioxidant, phenol antioxidant, alkylphenol polyoxyethylene ether emulsifier and part of desalted water, heating to 40-95 deg.C, shearing, emulsifying, dispersing, cooling to room temperature, adding water soluble polymer stabilizer and residual desalted water, and making into antioxidant dispersion liquid with average particle size less than 5.0 μm.
7. A terminator composition comprising the antioxidant dispersion liquid according to any one of claims 1 to 5, characterized in that: comprises an antioxidant dispersion and a hydroxylamine terminator.
8. A terminator composition according to claim 7, characterized in that: the hydroxylamine terminator is diethylhydroxylamine or N-isopropylhydroxylamine.
9. A terminator composition according to claim 7, characterized in that: the dosage of the hydroxylamine terminator is 0.01-0.20 percent of the mass of the vinyl chloride monomer.
10. Use of a terminator composition as claimed in claim 7, characterized in that: the method is used for vinyl chloride polymerization reaction by a suspension method.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107474167A (en) * | 2016-06-08 | 2017-12-15 | 中国石油化工股份有限公司 | Chloroethylene polymerization reaction terminating method |
| CN110760019A (en) * | 2018-07-25 | 2020-02-07 | 中国石油化工股份有限公司 | Vinyl chloride polymerization terminator, preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107474167A (en) * | 2016-06-08 | 2017-12-15 | 中国石油化工股份有限公司 | Chloroethylene polymerization reaction terminating method |
| CN110760019A (en) * | 2018-07-25 | 2020-02-07 | 中国石油化工股份有限公司 | Vinyl chloride polymerization terminator, preparation method and application thereof |
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