CN102321211A - Methods for preparing acrylate agglomerating agent and agglomerating polyacrylate latex by using acrylate agglomerating agent - Google Patents
Methods for preparing acrylate agglomerating agent and agglomerating polyacrylate latex by using acrylate agglomerating agent Download PDFInfo
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Abstract
The invention provides a method for preparing an acrylate agglomerating agent. The agglomerating agent comprises the following components in parts by mass: 10-12 parts of acrylate, 0.5-3.0 parts of unsaturated acid, 85-89 parts of de-ionized water, 0.03-0.08 part of initiating agent and 0.27-0.61 part of compound emulsifying agent; and the preparation method comprises the following steps of: pre-emulsifying all monomers and then putting into a reaction kettle; then putting the unsaturated acid; stirring and heating to 60-85 DEG C; adding the initiating agent; and performing heat preservation and a reaction for 2-6 hours. The invention also provides a method for agglomerating polyacrylate latex by using the acrylate agglomerating agent, and the agglomerating method comprises the following steps of: adding latex to be agglomerated and distilled water into a polymeric kettle according to a proportion; stirring while adding the agglomerating agent; stirring 10-60 minutes under a normal temperature and a normal pressure; and agglomerating for 10-60 minutes after adding and then discharging, wherein an agglomeration formula comprises the following components in parts by mass: 60-85 parts of polyacrylate latex, 5-20 parts of agglomerating agent and 15-30 parts of distilled water. The invention has the following advantages that: the raw material components of the agglomerating agent are simple and the acrylic monomer accounting for the total monomer amount is less; the agglomeration effect is good, the agglomeration period is short and the average particle diameter of the small particle latex is increased by over 4 times; and the agglomerating method is simple and convenient to operate.
Description
[technical field]
The present invention relates to the synthetic and big particle diameter polyacrylic ester latex preparation of the polymerization of ASA resin emulsion, polymer agglomerant, relate in particular to the agglomeration amplification that the esters of acrylic acid agglomerant prepares and be used for polyacrylic ester latex.
[background technology]
Polyacrylic ester latex is a kind of functional latex, is widely used in the aspects such as dip finishing agent of modified rubber, plastic toughening, coating, tackiness agent, paper and fabric, is developed rapidly in recent years.In modified rubber and plastic toughening, polyacrylic ester latex is as the basic latex of synthetic ASA resin, and its size influences the performance of final ASA rosin products.In order to obtain the product of high comprehensive performance, need the particle diameter of toughness reinforcing phase to reach more than the 200nm-500nm.
At present, what preparation ASA resinoid was the most frequently used is the emulsion graft polymerization method, and common emulsion method can only make the particle about 100nm, is difficult to reach design requirements.So,, small grain size latex is processed large grain size latex seems very necessary through hole enlargement.Being generally used for diameter enlarging method has a lot, like the cold method in the physical method, pressure application, mechanical mixing method; General chemical process is also arranged, like method of acetic acid; But the more satisfactory preparation method of effect is the polymer latex agglomeration technique.The agglomeration principle of polymer latex method is to utilize agglomerant to destroy the tensio-active agent of treating agglomerant, makes it be fused into bigger latex particle, thereby reaches the purpose that enlarges particle diameter.In recent years, continuous report relevant for the large grain size latex preparation method.Lanzhou branch office of PetroChina Company Limited. reported that the seed latex method prepared big particle diameter acrylate latex, but particle diameter has only about 120nm.Show that according to latest information with vinyl monomer or unsaturated acid ester and α, β unsaturated acid multipolymer is made agglomerant, can make the particle diameter of small-particle latex increase to 200-700nm.Lin Runxiong etc. have reported that the latex agglomeration technique synthesizes big Particle Butadiene-styrene Latex, can make median size reach 295nm; The agglomeration amplification that is used for butadiene latex with propylene ester class agglomerant was reported at Sichuan University and chemical research center, PetroChina Company Limited. Lanzhou jointly, and particle diameter can reach 400nm; Reports such as Lin Qingju are crossed and are utilized agglomerant can the styrene-butadiene latex of particle diameter for 150nm be increased to more than the 700nm; Daqing petrochemical was also once reported the agglomeration amplification that is used for styrene-butadiene latex with similar agglomerant, and was used for the big grain size product production of ABS600nm.
Recent research shows, with the latex agglomeration technique new technology of acrylic ester copolymerization latex agglomeration butadiene type latex, is representing functional emulsion development of new techniques direction.
Though for preparing agglomerant and being applied to the existing many reports of method that large grain size latex prepares, the composition of existing agglomerant is complicacy, function monomer is more; Acrylate content is less; Other component concentrations are more, and the raw material of some agglomerant needs oneself synthetic, and cost is higher; And raw material is not easy to obtain, and technology is difficult.In addition, utilize the esters of acrylic acid agglomerant to prepare the also rarely seen report of big particle diameter acrylate latex, and the particle diameter of the polyacrylic ester latex that general emulsion polymerisation process makes is little, and is difficult for realizing the particle diameter regulation and control, these all are unfavorable for industrializing implementation.
The present invention is in order to solve prior art problems, and research and preparation are used for the basic latex-big particle diameter polyacrylic ester latex of toughness reinforcing ASA resin and plastics.The synthetic rubber toughened resin of this type, the particle diameter of control rubber phase is crucial, generally will obtain the good ASA resin of over-all properties, requires the particle diameter of rubber phase to reach 200-500nm, so just can play reasonable toughening effect.For this reason, the present invention has studied the esters of acrylic acid agglomerant and the particle diameter of small particle size acrylate latex has been increased effect in line with goals research that is easy to industrializing implementation and the big particle diameter polyacrylic ester latex of preparation, to reach the particle diameter demand of preparation ASA resin.This agglomerant method should have characteristics such as controlled, the easy enforcement of particle diameter, agglomeration is effective, and can shorten the cycle of preparation ASA resin, is beneficial to industrializing implementation.
[summary of the invention]
One of technical problem to be solved by this invention is to provide a kind of preparation method who prepares the good acrylic ester high molecular type agglomerant of agglomeration effect.
Two of technical problem to be solved by this invention is to provide a kind of aforesaid propylene esters of gallic acid polymer agglomerant to be used for the agglomeration method of polyacrylic ester latex.
The present invention one of solves the problems of the technologies described above through following technical scheme: a kind of preparation method of esters of acrylic acid agglomerant is characterized in that: the active principle of described agglomerant is: by total mass is 100, and propenoate accounts for 10-12 part; Unsaturated acid accounts for 0.5-3.0 part, and deionized water accounts for 85-89, and initiator accounts for 0.03-0.08 part; Composite emulsifier accounts for 0.27-0.61 part, through the copolymer latex of emulsion polymerization prepared, is the esters of acrylic acid agglomerating latex by propenoate and unsaturated acid; With throwing in to reaction kettle after the preparatory emulsification of propenoate, unsaturated acid, composite emulsifier and deionized water; The monomeric charge order adopts and feeds intake stage by stage, and throws behind the unsaturated acid monomer, stirs and is warming up to 60-85 ℃; Add initiator, insulation reaction 2-6 hour.After reaction finished, emulsion presented oyster white.
Wherein, Propenoate is Bing Xisuandingzhi, ethyl propenoate or its mix monomer, and unsaturated acid is acrylic or methacrylic acid, and initiator is water soluble starters such as overcurrent acid potassium, ammonium persulphate; Composite emulsifier is that anionic emulsifier and nonionic emulsifying agent are that 1:2 ~ 2:1 is composite by mass ratio; Anionic emulsifier can be sodium lauryl sulphate, and X 2073, nonionic emulsifying agent are nonyl epoxy group(ing) ethers such as triton x-100.
The present invention through following technical scheme solve the problems of the technologies described above two: a kind of agglomeration method that aforesaid propylene esters of gallic acid agglomerant is used for polyacrylic ester latex; Comprise the steps: in polymeric kettle, to add in proportion to treat agglomerating latex and zero(ppm) water; Said agglomerating latex is a polyacrylic ester latex; Add agglomerant while stirring; Stir 10min-60min at normal temperatures and pressures, add discharging behind the continued agglomeration 10min-60min, can obtain median size is the above big particle diameter polyacrylic ester latex of 350nm.
By total mass is 100, and the agglomerant prescription that described esters of acrylic acid agglomerant is used for polyacrylic ester latex is:
Polyacrylic ester latex: 60-85 part;
Agglomerant: 5-20 part;
Zero(ppm) water: 10-30 part.
Advantage of the present invention is: replenished the deficiency of original technology, prepared a kind of esters of acrylic acid agglomerant, it is characterized in that with unsaturated dicarboxylic acid, esters of unsaturated carboxylic acids be raw material, under the initiator effect, synthesized binary or multiple copolymer through emulsion polymerization.This agglomerant staple is exactly basic latex--the acrylic ester monomer of synthetic ASA resin, and content occupies in component very at high proportion, makes like this that the performance of latex is unlikely to take place too big variation after the agglomeration.Agglomeration method provided by the invention can be according to the difference of used agglomerant consumption and former latex; Prepare the different esters of acrylic acid latex of size; And can prepare the big particle diameter polyacrylic ester latex of median size more than 350nm; Particle diameter increases to more than 4.3 times, and prepared latex particle size size has reached the particle diameter requirement of preparation ASA resin.This agglomerant preparation method has advantages such as controlled, the easy enforcement of particle diameter, agglomeration is effective, and can shorten the cycle of preparation ASA resin, is beneficial to industrializing implementation.
Compared with prior art, beneficial effect of the present invention is embodied in:
1. the feed composition of the agglomerant of the present invention's preparation is simple, is made up of acrylic ester monomer, acrylic monomer, composite emulsifier, deionized water, initiator, and wherein, composite emulsifier is combined by anionic emulsifier and nonionic emulsifying agent in proportion;
2. the agglomerant of the present invention preparation, mainly by the binary or the multiple copolymer of acrylic ester monomer and acrylic monomer, it is less that acrylic monomer accounts for the total monomer amount, is 0.5%-25%;
3. the agglomeration of the agglomerant of the present invention's preparation is effective, and the agglomeration cycle is short, can make the median size of small-particle latex increase more than 4 times in the short period of time;
4. agglomeration method of the present invention is simple, and the agglomeration mild condition is easy to operate, directly agglomerant is added drop-wise to and treats in the agglomerant, stirs 10-60min, and agglomeration is promptly accomplished, and this agglomeration process gets final product at normal temperatures and pressures;
5. agglomeration method of the present invention can realize that particle diameter is controlled, according to the agglomerant consumption with treat the different of agglomerant consumption, can prepare the latex of different-grain diameter, can prepare the latex of median size between 100nm-400nm;
6. the component that is fit to agglomeration method of the present invention is simple, and by agglomerant, treat that agglomerant and deionized water etc. form, proportioning is regulated and control easily.
[embodiment]
Below in conjunction with embodiment the present invention is done further description so that those skilled in the art can better understand the present invention and implementing, but the embodiment that lifts not conduct to qualification of the present invention.
One, a kind of preparation method of esters of acrylic acid agglomerant.
Embodiment 1: by total mass is 100, and the composition of esters of acrylic acid agglomerant and content are:
10 parts of n-butyl acrylates
3 parts in vinylformic acid
86.7 parts of deionized waters
0.03 part of initiator
0.27 part of composite emulsifier
Wherein, composite emulsifier is that sodium lauryl sulphate and triton x-100 combine for 1:1-1:2 in proportion.
The preparation method of agglomerant
By component and content, with throwing in to reaction kettle after the preparatory emulsification of n-butyl acrylate, vinylformic acid, composite emulsifier and zero(ppm) water, stir and be warming up to 70 ℃, add initiator, 70 ℃ of insulation reaction 4 hours.After reaction finished, emulsion presented oyster white.
Embodiment 2: by total mass is 100, and the composition of esters of acrylic acid agglomerant and content are:
11 parts of n-butyl acrylates
2 parts in vinylformic acid
86.6 parts of deionized waters
0.05 part of initiator
0.35 part of composite emulsifier
Wherein, composite emulsifier is that sodium lauryl sulphate and triton x-100 combine for 1:1-1:2 in proportion.
By component and content, with throwing in to reaction kettle after the preparatory emulsification of n-butyl acrylate, vinylformic acid, composite emulsifier and zero(ppm) water, stir and be warming up to 60 ℃, add initiator, 60 ℃ of insulation reaction 6 hours.After reaction finished, emulsion presented oyster white.
Embodiment 3: by total mass is 100, and the composition of esters of acrylic acid agglomerant and umber are:
12 parts of n-butyl acrylates
2.31 parts in vinylformic acid
85 parts of deionized waters
0.08 part of initiator
0.61 part of composite emulsifier
Wherein, composite emulsifier is that sodium lauryl sulphate and triton x-100 combine for 1:1-1:2 in proportion.
By component and content, with throwing in to reaction kettle after the preparatory emulsification of n-butyl acrylate, vinylformic acid, composite emulsifier and zero(ppm) water, stir and be warming up to 80 ℃, add initiator, 80 ℃ of insulation reaction 2 hours.After reaction finished, emulsion presented oyster white.
Embodiment 4: by total mass is 100, and the composition of esters of acrylic acid agglomerant and umber are:
10 parts of n-butyl acrylates
0.5 part in vinylformic acid
89 parts of deionized waters
0.06 part of initiator
0.44 part of composite emulsifier
Wherein, composite emulsifier is that sodium lauryl sulphate and triton x-100 combine for 1:1-1:2 in proportion.
By component and content, with throwing in to reaction kettle after the preparatory emulsification of n-butyl acrylate, vinylformic acid, composite emulsifier and zero(ppm) water, stir and be warming up to 75 ℃, add initiator, 75 ℃ of insulation reaction 3 hours.After reaction finished, emulsion presented oyster white.
Embodiment 5: by total mass is 100, and the composition of esters of acrylic acid agglomerant and umber are:
11.3 parts of ethyl propenoates
1.7 parts in vinylformic acid
86.6 parts of deionized waters
0.04 part of initiator
0.36 part of composite emulsifier
Wherein, composite emulsifier is that sodium lauryl sulphate and triton x-100 combine for 1:1-1:2 in proportion.
By component and content, with throwing in to reaction kettle after the preparatory emulsification of n-butyl acrylate, vinylformic acid, composite emulsifier and zero(ppm) water, stir and be warming up to 70 ℃, add initiator, 70 ℃ of insulation reaction 4 hours.After reaction finished, emulsion presented oyster white.
Embodiment 6: by total mass is 100, and the composition of esters of acrylic acid agglomerant and umber are:
Mix 10.85 parts of acrylate monomers
1.15 parts of vinylformic acid/methylacrylic acids
87.6 parts of deionized waters
0.07 part of initiator
0.33 part of composite emulsifier
Wherein, mix monomer be n-butyl acrylate and ethyl propenoate 1:2-2:1 is composite in proportion forms, composite emulsifier is that sodium lauryl sulphate and triton x-100 combine for 1:1-1:2 in proportion.
By component and content, with throwing in to reaction kettle after the preparatory emulsification of n-butyl acrylate, vinylformic acid, composite emulsifier and zero(ppm) water, stir and be warming up to 85 ℃, add initiator, 85 ℃ of temperature control reactions 4 hours.After reaction finished, emulsion presented oyster white.
Two, the agglomeration method that above-mentioned agglomerant is used for polyacrylic ester latex.
Embodiment 7: above-mentioned made agglomerant is used for the agglomeration process of butyl polyacrylate (PBA) or polyethyl acrylate (PEA), should may further comprise the steps:
By total mass is 100, and agglomerant composition and proportioning are following:
65 parts in PBA latex
5 parts of agglomerants
30 parts of zero(ppm) water
In polymeric kettle, add in proportion and treat that agglomerating latex and zero(ppm) water, said agglomerating latex are polyacrylic ester latex, add agglomerant while stirring, stir 10min at normal temperatures and pressures, discharging behind the agglomeration 60min after adding.
It is 356.4nm that reaction finishes back sampling analysis median size, and former latex median size is 84.96nm.
Embodiment 8: by total mass is 100, and agglomerant composition and proportioning are following:
70 parts in PBA latex
7 parts of agglomerants
23 parts of zero(ppm) water
In polymeric kettle, add in proportion and treat that agglomerating latex and zero(ppm) water, said agglomerating latex are polyacrylic ester latex, add agglomerant while stirring, stir 20min at normal temperatures and pressures, discharging behind the agglomeration 60min after adding.It is 365.4nm that reaction finishes back sampling analysis median size, and former latex median size is 84.96nm.
Embodiment 9: by total mass is 100, and agglomerant composition and proportioning are following:
65 parts in PBA latex
10 parts of agglomerants
25 parts of zero(ppm) water
In polymeric kettle, add in proportion and treat that agglomerating latex and zero(ppm) water, said agglomerating latex are polyacrylic ester latex, add agglomerant while stirring, stir 30min at normal temperatures and pressures, discharging behind the agglomeration 40min after adding.It is 320.2nm that reaction finishes back sampling analysis median size, and former latex median size is 84.96nm.
Embodiment 10: by total mass is 100, and agglomerant composition and proportioning are following:
85 parts in PBA latex
5 parts of agglomerants
10 parts of zero(ppm) water
In polymeric kettle, add in proportion and treat that agglomerating latex and zero(ppm) water, said agglomerating latex are polyacrylic ester latex, add agglomerant while stirring, stir 40min at normal temperatures and pressures, discharging behind the agglomeration 30min after adding.It is 345.4nm that reaction finishes back sampling analysis median size, and former latex median size is 84.96nm.
Embodiment 11: by total mass is 100, and agglomerant composition and proportioning are following:
60 parts in PBA latex
20 parts of agglomerants
20 parts of zero(ppm) water
In polymeric kettle, add in proportion and treat that agglomerating latex and zero(ppm) water, said agglomerating latex are polyacrylic ester latex, add agglomerant while stirring, stir 60min at normal temperatures and pressures, discharging behind the agglomeration 10min after adding.It is 320.6nm that reaction finishes back sampling analysis median size, and former latex median size is 84.96nm.
Though more than described embodiment of the present invention; But the technician who is familiar with the present technique field is to be understood that; We described concrete embodiment is illustrative; Rather than being used for qualification to scope of the present invention, those of ordinary skill in the art are in the modification and the variation of the equivalence of doing according to spirit of the present invention, all should be encompassed in the scope that claim of the present invention protects.
Claims (9)
1. the preparation method of an esters of acrylic acid agglomerant, it is characterized in that: the active principle of described agglomerant is: by total mass is 100, and propenoate accounts for 10-12 part; Unsaturated acid accounts for 0.5-3.0 part, and deionized water accounts for 85-89, and initiator accounts for 0.03-0.08 part; Composite emulsifier accounts for 0.27-0.61 part, and with throwing in to reaction kettle after the preparatory emulsification of propenoate, unsaturated acid, composite emulsifier and deionized water, the monomeric charge order adopts and feeds intake stage by stage; And throw behind the unsaturated acid monomer; Stirring is warming up to 60-85 ℃, adds initiator, insulation reaction 2-6 hour.
2. the preparation method of esters of acrylic acid agglomerant as claimed in claim 1 is characterized in that: wherein, propenoate is Bing Xisuandingzhi, ethyl propenoate or its mix monomer.
3. the preparation method of esters of acrylic acid agglomerant as claimed in claim 1 is characterized in that: unsaturated acid is acrylic or methacrylic acid.
4. the preparation method of esters of acrylic acid agglomerant as claimed in claim 1 is characterized in that: initiator is a water soluble starter.
5. the preparation method of esters of acrylic acid agglomerant as claimed in claim 4 is characterized in that: initiator is overcurrent acid potassium or ammonium persulphate.
6. the preparation method of esters of acrylic acid agglomerant as claimed in claim 1 is characterized in that: composite emulsifier is that anionic emulsifier and nonionic emulsifying agent are that 1:2 ~ 2:1 is composite by mass ratio.
7. the preparation method of esters of acrylic acid agglomerant as claimed in claim 6 is characterized in that: anionic emulsifier is sodium lauryl sulphate or X 2073, and nonionic emulsifying agent is a nonyl epoxy group(ing) ethers.
8. the preparation method of esters of acrylic acid agglomerant as claimed in claim 7 is characterized in that: nonionic emulsifying agent is a triton x-100.
9. one kind requires 1 to 8 each the esters of acrylic acid agglomerant of preparation to be used for the agglomeration method of polyacrylic ester latex the aforesaid right; It is characterized in that: comprise the steps: in polymeric kettle, to add in proportion to treat agglomerating latex and zero(ppm) water; The said agglomerating latex of treating is a polyacrylic ester latex; Add agglomerant while stirring, stir 10min-60min at normal temperatures and pressures, add discharging behind the agglomerant continued reaction 10min-60min; By total mass is 100, and the agglomerant prescription that described esters of acrylic acid agglomerant is used for polyacrylic ester latex is:
Polyacrylic ester latex: 60-85 part;
Agglomerant: 5-20 part;
Zero(ppm) water: 15-30 part.
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Cited By (5)
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| CN103242478A (en) * | 2013-05-17 | 2013-08-14 | 合肥工业大学 | Acrylate agglomerant and preparation method thereof, and method for modifying ASA (acrylonitrile-styrene-acrylate) resin with agglomerant |
| CN109897141A (en) * | 2019-04-08 | 2019-06-18 | 淮安市博彦土木工程科学研究院有限公司 | A kind of preparation method of the high-intensitive ASA resin of building materials |
| CN112661909A (en) * | 2019-05-05 | 2021-04-16 | 淮安市博彦土木工程科学研究院有限公司 | Preparation method of flame-retardant agglomerating agent for building material field |
| CN113583154A (en) * | 2021-09-07 | 2021-11-02 | 河北工业大学 | Preparation method of polyacrylate latex particles with large particle size |
| CN113754797A (en) * | 2021-08-27 | 2021-12-07 | 北方华锦化学工业股份有限公司 | Preparation method and application technology of polymer agglomerated latex |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103242478A (en) * | 2013-05-17 | 2013-08-14 | 合肥工业大学 | Acrylate agglomerant and preparation method thereof, and method for modifying ASA (acrylonitrile-styrene-acrylate) resin with agglomerant |
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| CN109897141A (en) * | 2019-04-08 | 2019-06-18 | 淮安市博彦土木工程科学研究院有限公司 | A kind of preparation method of the high-intensitive ASA resin of building materials |
| CN109897141B (en) * | 2019-04-08 | 2021-03-02 | 淮安市博彦土木工程科学研究院有限公司 | Preparation method of high-strength ASA resin for building materials |
| CN112661909A (en) * | 2019-05-05 | 2021-04-16 | 淮安市博彦土木工程科学研究院有限公司 | Preparation method of flame-retardant agglomerating agent for building material field |
| CN112661909B (en) * | 2019-05-05 | 2022-01-07 | 淮安市博彦土木工程科学研究院有限公司 | Preparation method of flame-retardant agglomerating agent for building material field |
| CN113754797A (en) * | 2021-08-27 | 2021-12-07 | 北方华锦化学工业股份有限公司 | Preparation method and application technology of polymer agglomerated latex |
| CN113583154A (en) * | 2021-09-07 | 2021-11-02 | 河北工业大学 | Preparation method of polyacrylate latex particles with large particle size |
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| CN102321211B (en) | 2016-04-27 |
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