CN115707719B - PVC resin polymerization dispersion auxiliary agent, preparation method and resin preparation method - Google Patents
PVC resin polymerization dispersion auxiliary agent, preparation method and resin preparation method Download PDFInfo
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Abstract
A PVC resin polymerization dispersion auxiliary agent, a preparation method and application thereof belong to the technical field of polyvinyl chloride polymerization auxiliary agents. The prior art adopts different methods to solve the problem of thermal aging of the resin. However, the effect of the use is not the same due to the difference of the performance of the auxiliary agent or the system. According to the application, 10 parts of water, 0.6-0.8 part of sodium dodecyl sulfate, 0.7-0.9 part of hexadecyl trimethyl ammonium bromide, 0.8-1.2 parts of dimethyl sulfoxide and 0.2-0.3 part of organic tin stabilizer are used, and a dispersion auxiliary agent is formed by matching a specific weight part of anionic surfactant, a specific weight part of cationic surfactant and a specific weight part of nonionic surfactant, and the organic tin stabilizer is added, so that the dispersion effect of a dispersing agent on other components is remarkably improved, meanwhile, the distribution uniformity of organic tin in PVC resin is also improved, the influence on an initiator is avoided, the reaction rate is ensured, and the ageing whiteness of the PVC resin is improved.
Description
Technical Field
A PVC resin polymerization dispersion auxiliary agent, a preparation method and a resin preparation method belong to the technical field of polyvinyl chloride polymerization auxiliary agents.
Background
The heat aging whiteness of the PVC resin by the suspension method is a very important item in various indexes of PVC, and directly influences the appearance aging resistance of PVC products and the service life of the products. There are many factors affecting the whiteness of PVC resins, and different methods have been adopted in the prior art to solve the heat aging problem of the resins. Generally, an auxiliary agent is added in the polymerization to improve the ageing resistance of the resin.
The method commonly adopted in the common technical means is to add white additives such as titanium dioxide, but in the method, the compatibility of the added inorganic additives and a resin matrix is generally poor, the conditions such as precipitation and separation are easy to occur along with the time increase, and the organic additives can influence the polymerization reaction on one hand and can cause the conditions such as oxidative yellowing on the other hand, so that the method has poor stability.
Chinese patent CN02807882.9 is used in a method of aqueous suspension polymerization of vinyl chloride, the polymerization initiator contains at least one compound selected from dialkyl peroxydicarbonates, t-alkyl peroxyalkanoates and diacyl peroxides, and nitroxide-type stable free radicals are used as polymerization terminators. The resin thus obtained has a good white color, but the whiteness of the resin after aging is significantly reduced.
Chinese patent CN201610577253.4 provides a method for improving the ageing whiteness of PVC resins. The solid hindered phenol anti-aging agent emulsified by the emulsifier at a certain temperature is used for carrying out anti-aging treatment on the toughening latex, and then the toughening latex is added into PVC slurry to prepare the toughening PVC resin under the action of the flocculant. The ageing whiteness of the PVC resin prepared from the toughened latex subjected to the anti-ageing treatment is greatly improved, and the thermal stability and the processing stability of the toughened PVC resin are also effectively improved. The process is complex, has high control difficulty and is not easy for industrial production.
Disclosure of Invention
The technical problems to be solved by the application are as follows: overcomes the defects of the prior art, and provides a PVC resin polymerization dispersion auxiliary agent with good dispersion performance, a preparation method and application thereof, wherein the PVC resin polymerization dispersion auxiliary agent can effectively improve the ageing whiteness of PVC resin.
The technical scheme adopted for solving the technical problems is as follows: the PVC resin polymerization dispersion auxiliary agent is characterized in that: comprises the following components in parts by weight: 10 parts of water, 0.6-0.8 part of sodium dodecyl sulfate, 0.7-0.9 part of hexadecyl trimethyl ammonium bromide, 0.8-1.2 parts of dimethyl sulfoxide and 0.2-0.3 part of organic tin stabilizer.
Sodium dodecyl sulfate is generally used as an anionic surfactant, cetyl trimethyl ammonium bromide is generally used as a cationic surfactant, and in the field of PVC resin polymerization, the anionic surfactant or the cationic surfactant is generally considered to react to generate precipitate, but the inventor finds that when sodium dodecyl sulfate and cetyl trimethyl ammonium bromide are combined, the nonionic surfactant dimethyl sulfoxide is added to well overcome the mutual reaction problem of the anionic surfactant and the cationic surfactant, and the dispersing effect of the dispersing agent is obviously enhanced, and by utilizing the characteristic of the dispersing aid, the dispersing effect of the organotin stabilizer is increased, and the effects of improving the ageing whiteness and the heat stability of the PVC resin are synchronously realized.
Preferably, the composition comprises the following components in parts by weight: 10 parts of water, 0.7 part of sodium dodecyl sulfate, 0.8 part of hexadecyl trimethyl ammonium bromide, 1 part of dimethyl sulfoxide and 0.3 part of organic tin stabilizer.
The preferable dispersing auxiliary agent in parts by weight has stronger matching effect with the organotin stabilizer and the dispersing agent, the dispersing effect is stronger, and finally the prepared PVC has higher ageing whiteness.
Preferably, the organotin stabilizer is organotin maleate or organotin fatty carboxylate.
Preferably, the organotin heat stabilizer has a stronger effect of improving the heat stability of the PVC resin under the dispersion aid system.
The preparation method of the PVC resin polymerization dispersion auxiliary agent is characterized by comprising the following steps of: and weighing the raw materials according to the weight part ratio of the PVC resin polymerization dispersing auxiliary, heating to 45-50 ℃, and shearing at a high speed for 40-80 min to obtain the PVC resin polymerization dispersing auxiliary.
The PVC resin polymerization dispersion auxiliary agent prepared by the preferred method has more stable property, long storage time, difficult precipitation of an internal organotin stabilizer and better effect of improving ageing whiteness after being added into the PVC resin.
Preferably, the high-speed shearing is performed in an emulsifying machine at a rotating speed of 5500 r/min.
A preparation method of PVC resin is characterized in that: in PVC resin polymerization, after the PVC resin polymerization dispersion auxiliary agent and the dispersing agent are uniformly mixed, adding the mixture into a reaction system when the polymerization VCM monomer conversion rate reaches 60-70%, and preparing the PVC resin.
The polymerization dispersion auxiliary agent and part of dispersing agent are added in the middle and later stages of vinyl chloride polymerization, so that on one hand, the premature introduction of the organotin stabilizer can be avoided, the influence of the organotin stabilizer on the polymerization reaction caused by the attraction of free radicals of an initiator is avoided, and on the other hand, the dispersion auxiliary agent and the dispersing agent are mixed in advance, so that the dispersion effect of the dispersing agent and the organotin stabilizer can be improved, and due to the special effect of the surfactant in the dispersion auxiliary agent, the organotin stabilizer can be added in the polymerization process, and compared with the addition of the surfactant when the reaction is terminated, the dispersion effect of the organotin stabilizer can be improved, so that the ageing whiteness of PVC resin is improved.
Preferably, the preparation of the PVC resin comprises the following steps:
1) Adding deionized water, part of dispersing agent and initiator into a reaction container, vacuumizing, adding vinyl chloride monomer, stirring and heating to the reaction temperature;
2) When the conversion rate of vinyl chloride monomer reaches 60-70%, adding the PVC resin polymerization dispersion auxiliary agent and the mixed solution of the residual dispersing agent for continuous reaction;
3) Adding a terminator to the reaction end point, uniformly stirring, cooling, centrifugally dehydrating, drying and sieving at 55-65 ℃ to obtain PVC resin;
wherein, part of the dispersing agent in the step 1) is 0.8-0.9 times of the total consumption of the dispersing agent.
When the reaction starts, part of dispersing agent is added to ensure the dispersing effect of each auxiliary agent and vinyl chloride monomer in the initial stage of the reaction, and the rest of dispersing agent is used for being matched with the dispersing auxiliary agent to improve the dispersing effect, especially the dispersing effect of the organotin stabilizer.
Preferably, the PVC resin comprises, by weight, 100 parts of vinyl chloride monomer, 170 parts of deionized water, 1-6 parts of initiator, 1-6 parts of dispersant and 3 parts of terminator;
the PVC resin polymerization dispersing agent comprises, by weight, 90-100 parts of a dispersing agent and 5-10 parts of the PVC resin polymerization dispersing agent.
The preferable weight part collocation can fully ensure the dispersion assisting effect of the dispersion auxiliary agent and improve the ageing whiteness.
Preferably, the initiator is one or a mixture of a plurality of the diethyl hexyl peroxydicarbonate EHP, the tert-amyl peroxypivalate TAPP and the tert-hexyl peroxypivalate PV70 in any proportion.
Further preferably, the initiator is selected from diethyl hexyl peroxydicarbonate EHP and t-hexyl peroxypivalate PV70 according to a weight ratio of 1:0.8 to 0.9.
The optimized initiator has better matching effect with each surfactant and the organic tin stabilizer in the dispersing auxiliary, further avoids the effect of inhibiting reaction after the organic tin stabilizer is added into a reaction system, reduces mutual influence, ensures the polymerization effect and can improve certain ageing whiteness.
Preferably, the dispersing agent is polyvinyl alcohol PVA80 and hydroxypropyl methyl cellulose E50 according to the weight ratio of 1-2: 1 by weight ratio.
The preferable composite dispersing agent is more suitable for being matched with a surfactant in a dispersing auxiliary agent, so that the dispersion assisting effect is improved, and the dispersion effect of the organic tin stabilizer is improved.
Compared with the prior art, the application has the following beneficial effects: the special coordination action among three specific anionic surfactants, cationic surfactants and nonionic surfactants is found, and the organic tin stabilizer is matched, so that the dispersing effect of the dispersing agent on other components is remarkably improved, meanwhile, the distribution uniformity of organic tin in the PVC resin is improved, the influence on an initiator is avoided, the reaction rate is ensured, and the heat-resistant stability of the final PVC resin such as ageing whiteness is improved.
Detailed Description
The present application will be further described with reference to the following examples, with example 1 being the best mode of carrying out the application.
Example 1
A PVC resin polymerization dispersion aid comprises 10g of water, 0.7g of anionic surfactant sodium dodecyl sulfate, 0.8g of cationic surfactant cetyl trimethyl ammonium bromide, 1g of nonionic surfactant dimethyl sulfoxide and 0.3g of organotin maleate.
The preparation process of PVC resin polymerization dispersing assistant includes the steps of weighing the materials, heating to 45 deg.c, stirring, shearing at 5500r/min in an emulsifying machine for 60min to obtain homogeneous and stable PVC resin polymerization dispersing assistant.
A preparation method of PVC resin comprises the following steps:
1) 2450g of desalted water, 0.45g of diethyl hexyl peroxydicarbonate EHP, 0.45g of tert-amyl peroxypivalate TAPP,0.5g of polyvinyl alcohol PVA80 and 0.3g of hydroxypropyl methylcellulose E50 are added into a stainless steel reaction kettle, 1300g of vinyl chloride monomer is added after vacuum pumping, stirring is carried out for 15 minutes at normal temperature, timing is started after the temperature is raised to the specified reaction temperature, and the temperature control range is 58.1+/-0.5 ℃.
2) When the pressure drop value in the kettle reaches 0.16MPa, 0.08g of PVA80, 0.06g of hydroxypropyl methylcellulose E50 and 0.05g of PVC resin polymerization dispersion auxiliary agent are added for continuous reaction.
3) When the pressure drop value in the kettle reaches 0.20MPa, 0.16g of terminator DEHA is added, and the kettle is emptied and discharged after stirring for 5 minutes.
4) After the polymerization reaction operation is completed, the wet material obtained by centrifugal dehydration is dried in a blast drying oven at 60+/-5 ℃ for 6 hours, and the obtained dry powder is sieved by a 10-mesh sieve (with the sieve pore diameter of 1.65 mm) to obtain the final product PVC resin.
Example 2
On the basis of example 1, in the preparation method of the PVC resin, the step 1) is as follows:
1) 2450g of desalted water, 0.45g of diethyl hexyl peroxydicarbonate EHP, 0.43g of tertbutyl peroxypivalate PV70,0.5g of polyvinyl alcohol PVA80 and 0.3g of hydroxypropyl methylcellulose E50 are added into a stainless steel reaction kettle, 1300g of vinyl chloride monomer is added after vacuum pumping, stirring is carried out for 15 minutes at normal temperature, timing is started after the temperature is raised to the specified reaction temperature, and the temperature control range is 58.1+/-0.5 ℃.
The final PVC resin was prepared under the same conditions as in example 1.
Example 3
On the basis of the embodiment 1, the organotin maleate in the PVC resin polymerization dispersing auxiliary is replaced by organotin fatty carboxylate.
In the preparation method of the PVC resin, the step 1) is as follows:
1) 2450g of desalted water, 0.45g of diethyl hexyl peroxydicarbonate EHP, 0.42g of tertbutyl peroxypivalate PV70,0.5g of polyvinyl alcohol PVA80 and 0.3g of hydroxypropyl methylcellulose E50 are added into a stainless steel reaction kettle, 1300g of vinyl chloride monomer is added after vacuum pumping, stirring is carried out for 15 minutes at normal temperature, timing is started after the temperature is raised to the specified reaction temperature, and the temperature control range is 58.1+/-0.5 ℃.
The final PVC resin was prepared under the same conditions as in example 1.
Example 4
Based on the example 1, 0.08g of polyvinyl alcohol PVA80, 0.06g of hydroxypropyl methyl cellulose E50 and 0.05g of PVC resin polymerization dispersion auxiliary agent in the step 2) are added together with other components in the step 1) in the preparation method of the PVC resin, and simultaneously participate in the reaction.
The final PVC resin was prepared under the same conditions as in example 1.
Example 5
On the basis of example 1, step 2) in the preparation method of the PVC resin is set as follows:
2) When the pressure drop value in the kettle reaches 0.12MPa, 0.08g of PVA80, 0.06g of hydroxypropyl methylcellulose E50 and 0.05g of PVC resin polymerization dispersion auxiliary agent are added for continuous reaction.
Comparative example 1
On the basis of example 1, the composition of the PVC resin polymerization dispersion auxiliary agent is as follows:
comprises 10g of deionized water, 1g of anionic surfactant sodium dodecyl sulfate, 1.2g of cationic surfactant cetyl trimethyl ammonium bromide and 0.3g of organotin maleate.
The final PVC resin was prepared under the same conditions as in example 1.
Comparative example 2
A PVC resin polymerization dispersion aid, a preparation method and a resin preparation method, based on example 1, the composition of the PVC resin polymerization dispersion aid based on example 1 is set as follows:
comprises 10g of deionized water, 1.1g of cationic surfactant cetyl trimethyl ammonium bromide, 1.4g of nonionic surfactant dimethyl sulfoxide and 0.3g of organotin maleate.
The final PVC resin was prepared under the same conditions as in example 1.
Comparative example 3
A PVC resin polymerization dispersion aid, a preparation method and a resin preparation method, based on example 1, the composition of the PVC resin polymerization dispersion aid based on example 1 is set as follows:
comprises 10g of deionized water, 1.1g of anionic surfactant sodium dodecyl sulfate, 1.4g of nonionic surfactant dimethyl sulfoxide and 0.3g of organotin maleate.
The final PVC resin was prepared under the same conditions as in example 1.
Comparative example 4
On the basis of example 1, the composition of the PVC resin polymerization dispersion auxiliary agent is as follows:
comprises 10g of deionized water, 0.7g of anionic surfactant sodium dodecyl sulfate, 0.8g of cationic surfactant cetyl trimethyl ammonium bromide, 1g of nonionic surface alkylphenol ethoxylate and 0.3g of organotin maleate.
Comparative example 5
On the basis of example 1, the composition of the PVC resin polymerization dispersion auxiliary agent is as follows:
comprises 10g of deionized water, 0.7g of anionic surfactant alkylbenzene sulfonate, 0.8g of cationic surfactant cetyl trimethyl ammonium bromide, 1g of nonionic surfactant dimethyl sulfoxide and 0.3g of organotin maleate.
Comparative example 6
On the basis of example 1, the composition of the PVC resin polymerization dispersion auxiliary agent is as follows:
comprises 10g of deionized water, 0.7g of anionic surfactant sodium dodecyl sulfate, 0.8g of cationic surfactant cetyl trimethyl ammonium bromide, 0.5g of nonionic surfactant dimethyl sulfoxide and 0.3g of organotin maleate.
Performance testing
The PVC resin prepared above is subjected to performance test, and the test standard is as follows:
(1) Average degree of polymerization: according to GB/T5761-2006 (appendix A);
(2) Apparent density: according to GB/T20022-2005 test;
(3) Plasticizer absorption of 100g resin: according to GB/T3400-2002 test;
(4) Number of "fish eyes": according to GB/T4611-2008 test;
(5) Whiteness (160 ℃,10 min): according to GB/T15595-2008 test;
(6) Polymerization yield: weight method, ratio of resin mass to vinyl chloride mass in the polymerization system;
(7) Tensile properties: according to GB/T1040.3-2006 test, the stretching speed is 250mm/min;
(8) Heat aging properties (cable material): according to GB/T8815-2008 test;
(9) Yellow index: the test is carried out according to the national standard HG/T3862-2006 (the original national standard GB/T2409-1980 is invalidated, and the 3862 standard adopted at present is consistent with the original standard content);
(10) Transmittance and haze: the test is carried out according to national standard GB/T2410-2008.
The results of the examples are shown in Table 1 below and the results of the comparative examples are shown in Table 2 below.
Table 1 example performance test results
。
Table 2 comparative example performance test results
。
From the test results in tables 1 and 2, it can be seen that only specific anionic surfactant sodium dodecyl sulfate, cationic surfactant cetyl trimethyl ammonium bromide and nonionic surfactant dimethyl sulfoxide can obtain good dispersion assisting and ageing whiteness improving effects. Wherein, the surface active effect of the three-phase dispersion auxiliary agent can be broken due to the fact that a certain component is too little or missing, the organic tin stabilizer is excessively concentrated, free radicals of the initiator are attracted, the initiating effect of the initiator is reduced, and the performance of the PVC resin is reduced.
The above description is only a preferred embodiment of the present application, and is not intended to limit the application in any way, and any person skilled in the art may make modifications or alterations to the disclosed technical content to the equivalent embodiments. However, any simple modification, equivalent variation and variation of the above embodiments according to the technical substance of the present application still fall within the protection scope of the technical solution of the present application.
Claims (7)
1. A preparation method of PVC resin is characterized in that: the method comprises the following steps:
1) Adding deionized water, part of dispersing agent and initiator into a reaction container, vacuumizing, adding vinyl chloride monomer, stirring and heating to the reaction temperature;
2) When the conversion rate of vinyl chloride monomer reaches 60-70%, adding a PVC resin polymerization dispersion auxiliary agent and a mixed solution of the residual dispersing agent for continuous reaction;
3) Adding a terminator to the reaction end point, uniformly stirring, cooling, centrifugally dehydrating, drying and sieving at 55-65 ℃ to obtain PVC resin;
the PVC resin polymerization dispersion auxiliary agent comprises the following components in parts by weight: 10 parts of water, 0.6-0.8 part of sodium dodecyl sulfate, 0.7-0.9 part of hexadecyl trimethyl ammonium bromide, 0.8-1.2 parts of dimethyl sulfoxide and 0.2-0.3 part of organic tin stabilizer;
in PVC resin polymerization, after the PVC resin polymerization dispersing aid and the dispersing agent are uniformly mixed, adding the mixture into a reaction system when the conversion rate of the polymerized vinyl chloride monomer reaches 60-70%, so as to prepare PVC resin;
wherein, part of the dispersing agent in the step 1) is 0.8-0.9 times of the total consumption of the dispersing agent;
the dispersing agent is prepared from polyvinyl alcohol PVA80 and hydroxypropyl methyl cellulose E50 according to a ratio of 1-2: 1 by weight ratio.
2. The method for producing a PVC resin according to claim 1, wherein: comprises the following components in parts by weight: 10 parts of water, 0.7 part of sodium dodecyl sulfate, 0.8 part of hexadecyl trimethyl ammonium bromide, 1 part of dimethyl sulfoxide and 0.3 part of organic tin stabilizer.
3. The method for producing a PVC resin according to claim 1, wherein: the organotin stabilizer is organotin maleate or organotin fatty carboxylate.
4. A method for preparing a PVC resin according to any one of claims 1 to 3, characterized in that: the preparation method of the PVC resin polymerization dispersion auxiliary agent comprises the following steps:
and weighing the raw materials according to the weight part ratio of the PVC resin polymerization dispersing auxiliary, heating to 45-50 ℃, and shearing for 40-80 min to obtain the PVC resin polymerization dispersing auxiliary.
5. The method for producing a PVC resin according to claim 4, wherein: the shearing is high-speed shearing in an emulsifying machine at a rotating speed of 5500 r/min.
6. The method for producing a PVC resin according to claim 1, wherein: the PVC resin comprises 100 parts of vinyl chloride monomer, 170 parts of deionized water, 1-6 parts of initiator, 1-6 parts of dispersant system and 3 parts of terminator in parts by weight;
the dispersing agent system comprises 90-100 parts of dispersing agent and 5-10 parts of PVC resin polymerization dispersing auxiliary agent as claimed in any one of claims 1-3.
7. The method for producing a PVC resin according to claim 1, wherein: the initiator is one or a mixture of a plurality of diethyl hexyl peroxydicarbonate, tert-amyl peroxypivalate and tert-hexyl peroxypivalate in any proportion.
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