CN103374136A - Preparation method of anti-drip agent based on electrostatic adsorption and wrapping - Google Patents
Preparation method of anti-drip agent based on electrostatic adsorption and wrapping Download PDFInfo
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- CN103374136A CN103374136A CN 201210123799 CN201210123799A CN103374136A CN 103374136 A CN103374136 A CN 103374136A CN 201210123799 CN201210123799 CN 201210123799 CN 201210123799 A CN201210123799 A CN 201210123799A CN 103374136 A CN103374136 A CN 103374136A
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Abstract
The invention relates to a preparation method of an anti-drip agent based on the electrostatic adsorption and wrapping. The preparation method comprises the following steps of: 1, measuring two reaction monomers according to a ratio of 4:1, adding 1% of cation surface active agent, and carrying out the pre-emulsification to obtain pre-emulsion; 2, adding the pre-emulsion into a round-bottom flask, adding deionized water which is twice of the total quantity of the monomers, uniformly mixing the deionized water with the pre-emulsion, maintaining rotating speed at 120 r/min, carrying out a polymerization reaction for 6 to 8h at the temperature of 70 to 80 DEG C, and cooling reaction products to the room temperature after the reaction to obtain polymer emulsion; 3, adding partial polymer emulsion into a polytetrafluoroethylene diffusion solution of the same volume, and heating and stirring the mixture to obtain a great amount of precipitate; and 4, carrying out vacuum filtration to the precipitate, washing the emulsifier through a given method, and drying and pulverizing the precipitate to obtain the anti-drip agent. By adopting the method, the stable polymer emulsion can be prepared, simplicity in operation can be realized, the cost is low, and the preparation method has the advantages that the polymerization process is stable and the product quality is consistent.
Description
Technical field:
The present invention relates to a kind of anti-dripping agent preparation method, be specifically related to a kind of anti-dripping agent preparation method based on the electrostatic adhesion parcel.
Background technology:
Thermoplastic material has lightly, be convenient to the advantages such as manufacturing and suitability for industrialized production, every aspect in our daily productive life has its figure, brought huge power for human development, but because thermoplastic material easy firing, easy softening transform is heated, even drop, needing in process of production to add fire retardant makes it have the larger scope of application, but fire retardant can only reduce the probability of its burning, well do not solve the problem that hangs after its temperature distortion, in order to reach the performance requriements of anti-drippage, some have the high molecular polymer that is subjected to heat shrinkability characteristic and have been used to improve the drippage problem of thermoplastic material.As disclosing in the United States Patent (USP) 4463130,5109044 etc. polytetrafluoroethylene granule is added among the synthetic resins PC/ABS as anti-dripping agent, improved the effect of its anti-drippage.But tetrafluoroethylene dispersed relatively poor causes being difficult for adding, in order to improve the dispersiveness of polytetrafluoroethylene granule, can by at polytetrafluoroethylene granule parcel one layer of polymeric to improve its surface property, reach preferably dispersing property.
Summary of the invention:
The purpose of this invention is to provide a kind of anti-dripping agent preparation method based on the electrostatic adhesion parcel, it can prepare more stable polymer emulsion, and is simple to operate, and cost is low, and it is stable to have polymerization process, the equal first-class advantage of quality product.
In order to solve the existing problem of background technology, the present invention is by the following technical solutions: its preparation method is: after 1, certain two kinds of reaction monomers being measured according to 4: 1 ratio, the cats product of adding 1% carries out pre-emulsification, obtains pre-emulsion; 2, pre-emulsion is added in the round-bottomed flask, add the deionized water that is about 2 times of monomer total amounts, after mixing, keep rotating speed 120r/min, carried out polyreaction 6-8 hour at 70-80 ℃, be cooled to room temperature after reaction finishes and obtain polymer emulsion; 3, the partial polymer emulsion is added in the polytetrafluoroethyldispersion dispersion of equivalent, precipitated in a large number after the heated and stirred; 4, precipitation is carried out decompress filter, with certain method flush away emulsifying agent wherein, oven dry is pulverized, and obtains described anti-dripping agent.
Described polymer monomer is one of following or wherein two or more mixing: methyl methacrylate, vinylbenzene, divinyl, butyl methacrylate, vinyl cyanide, methacrylic acid;
Described cats product and initiator can be selected according to the polymer monomer kind, and cats product is one of following or wherein two or more mixing: dodecyl benzyl dimethyl ammonium chloride, palmityl trimethyl ammonium chloride, cetyl trimethylammonium bromide, octadecyl trimethyl ammonium chloride.
Described initiator is one of following or wherein two or more mixing: Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile), benzoyl peroxide, Potassium Persulphate, ammonium persulphate.
The present invention has following beneficial effect:
1, adopts the monomer of interrupter method to add mode, simplified polymerization process, improved W-response efficient.
2, by using cationic emulsifier, so that PTFE and monomer produce electrostatic adsorption, increased both bonding forces, thereby further strengthened when reacting and the stability of the polymer emulsion that makes after the reaction.
3, adopt the altogether method of cohesion, further improved the stability of polyreaction and the efficient of whole experimentation.
Embodiment:
This embodiment is by the following technical solutions: after 1, certain two kinds of reaction monomers being measured according to 4: 1 ratio, add 1% cats product, carry out pre-emulsification, obtain pre-emulsion; 2, pre-emulsion is added in the round-bottomed flask, add the deionized water that is about 2 times of monomer total amounts, after mixing, keep rotating speed 120r/min, carried out polyreaction 6-8 hour at 70-80 ℃, be cooled to room temperature after reaction finishes and obtain polymer emulsion; 3, the partial polymer emulsion is added in the polytetrafluoroethyldispersion dispersion of equivalent, precipitated in a large number after the heated and stirred; 4, precipitation is carried out decompress filter, with certain method flush away emulsifying agent wherein, oven dry is pulverized, and obtains described anti-dripping agent.
Described polymer monomer is one of following or wherein two or more mixing: methyl methacrylate, vinylbenzene, divinyl, butyl methacrylate, vinyl cyanide, methacrylic acid;
Described cats product and initiator can be selected according to the polymer monomer kind, and cats product is one of following or wherein two or more mixing: dodecyl benzyl dimethyl ammonium chloride, palmityl trimethyl ammonium chloride, cetyl trimethylammonium bromide, octadecyl trimethyl ammonium chloride.
Described initiator is one of following or wherein two or more mixing: Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile), benzoyl peroxide, Potassium Persulphate, ammonium persulphate.
The present invention has following beneficial effect:
1, adopts the monomer of interrupter method to add mode, simplified polymerization process, improved W-response efficient.
2, by using cationic emulsifier, so that PTFE and monomer produce electrostatic adsorption, increased both bonding forces, thereby further strengthened when reacting and the stability of the polymer emulsion that makes after the reaction.
3, adopt the altogether method of cohesion, further improved the stability of polyreaction and the efficient of whole experimentation.
Embodiment 1:
1, takes by weighing 0.1g dodecyl benzyl dimethyl ammonium chloride and 0.05g palmityl trimethyl ammonium chloride, 19.2g vinylbenzene (St) and 4.8g vinyl cyanide (An) add a certain amount of distilled water, add in the 500ml flask, magnetic agitation 30min makes pre-emulsion.
2, pre-emulsion is added in the round-bottomed flask, add 0.05g Diisopropyl azodicarboxylate (AIBN) again, 70 ℃ of isothermal reactions keep 120r/min.Behind the reaction 2h, be warming up to 75 ℃, continue to add an amount of initiator (AIBN), improve monomer conversion, reaction 4h, total reaction time is 6h.
3, take by weighing the polymer emulsion of 40mlPTFE dispersion liquid and equivalent, be heated to 90 ℃, add the acetic acid solution of 1mol/L and the MgSO of 1mol/L
4Solution is precipitated after the stirring in a large number.
4, precipitation is carried out decompress filter, and repeatedly wash filter residue with hot water, flush away emulsifying agent wherein filters, and after the oven dry, pulverizes, and obtains monomer conversion and be 82.3% anti-dripping agent.
Embodiment 2:
1, takes by weighing 0.1g dodecyl benzyl dimethyl ammonium chloride and 0.05g palmityl trimethyl ammonium chloride, 19.2g vinylbenzene (St) and 4.8g vinyl cyanide (An) add a certain amount of distilled water, add in the 500ml flask, magnetic agitation 30min makes pre-emulsion.
2, pre-emulsion is added in the round-bottomed flask, add 0.05g Potassium Persulphate (KPS) again, 70 ℃ of isothermal reactions keep 120r/min.Behind the reaction 2h, be warming up to 75 ℃, continue to add an amount of initiator (KPS), improve monomer conversion, reaction 4h, total reaction time is 6h.
3, take by weighing the polymer emulsion of 40mlPTFE dispersion liquid and equivalent, be heated to 90 ℃, add the acetic acid solution of 1mol/L and the MgSO of 1mol/L
4Solution is precipitated after the stirring in a large number.
4, precipitation is carried out decompress filter, and repeatedly wash filter residue with hot water, flush away emulsifying agent wherein filters, and after the oven dry, pulverizes, and obtains monomer conversion and be 84.5% anti-dripping agent.
Embodiment 3:
1, takes by weighing 0.2g dodecyl benzyl dimethyl ammonium chloride and 0.1g palmityl trimethyl ammonium chloride, 57.6g vinylbenzene (St) and 14.4g vinyl cyanide (An) add a certain amount of distilled water, add in the 500ml flask, magnetic agitation 30min makes pre-emulsion.
2, pre-emulsion is added in the round-bottomed flask, add 0.25g Potassium Persulphate (KPS) again, 70 ℃ of isothermal reactions keep 120r/min.Behind the reaction 2h, be warming up to 75 ℃, continue to add an amount of initiator (KPS), improve monomer conversion, reaction 4h, total reaction time is 6h.
3, take by weighing the polymer emulsion of 120mlPTFE dispersion liquid and equivalent, be heated to 90 ℃, add the acetic acid solution of 1mol/L and the MgSO of 1mol/L
4Solution is precipitated after the stirring in a large number.
4, precipitation is carried out decompress filter, and repeatedly wash filter residue with hot water, flush away emulsifying agent wherein filters, and after the oven dry, pulverizes, and obtains monomer conversion and be 83.6% anti-dripping agent.
Embodiment 4:
1, takes by weighing 0.2g dodecyl benzyl dimethyl ammonium chloride and 0.1g palmityl trimethyl ammonium chloride, 19.2g vinylbenzene (St) and 4.8g vinyl cyanide (An) add a certain amount of distilled water, add in the 500ml flask, magnetic agitation 30min makes pre-emulsion.
2, pre-emulsion is added in the round-bottomed flask, add 0.5g Potassium Persulphate (KPS) again, 70 ℃ of isothermal reactions keep 120r/min.Behind the reaction 2h, be warming up to 75 ℃, continue to add an amount of initiator (KPS), improve monomer conversion, reaction 4h, total reaction time is 6h.
3, take by weighing the polymer emulsion of 40mlPTFE dispersion liquid and equivalent, be heated to 90 ℃, add the acetic acid solution of 1mol/L and the MgSO of 1mol/L
4Solution is precipitated after the stirring in a large number.
4, precipitation is carried out decompress filter, and repeatedly wash filter residue with hot water, flush away emulsifying agent wherein filters, and after the oven dry, pulverizes, and obtains monomer conversion and be 88.9% anti-dripping agent.
Embodiment 5:
1, takes by weighing 0.5g dodecyl benzyl dimethyl ammonium chloride and 0.25g palmityl trimethyl ammonium chloride, 69.12g vinylbenzene (St) and 17.28g vinyl cyanide (An) add a certain amount of distilled water, add in the 500ml flask, magnetic agitation 30min makes pre-emulsion.
2, pre-emulsion is added in the round-bottomed flask, add 0.6g Potassium Persulphate (KPS) again, 70 ℃ of isothermal reactions keep 120r/min.Behind the reaction 2h, be warming up to 75 ℃, continue to add an amount of initiator (KPS), improve monomer conversion, reaction 4h, total reaction time is 6h.
3, take by weighing the polymer emulsion of 120mlPTFE dispersion liquid and equivalent, be heated to 90 ℃, add the acetic acid solution of 1mol/L and the MgSO of 1mol/L
4Solution is precipitated after the stirring in a large number.
4, precipitation is carried out decompress filter, and repeatedly wash filter residue with hot water, flush away emulsifying agent wherein filters, and after the oven dry, pulverizes, and obtains monomer conversion and be 90.3% anti-dripping agent.
Embodiment 6:
1, takes by weighing 0.5g dodecyl benzyl dimethyl ammonium chloride and 0.25g palmityl trimethyl ammonium chloride, 69.12g vinylbenzene (St) and 17.28g vinyl cyanide (An) add a certain amount of distilled water, add in the 500ml flask, magnetic agitation 30min makes pre-emulsion.
2, pre-emulsion is added in the round-bottomed flask, add 0.7g Potassium Persulphate (KPS) again, 70 ℃ of isothermal reactions keep 120r/min.Behind the reaction 2h, be warming up to 75 ℃, continue to add an amount of initiator (KPS), improve monomer conversion, reaction 4h, total reaction time is 6h.
3, take by weighing the polymer emulsion of 120mlPTFE dispersion liquid and equivalent, be heated to 90 ℃, add the acetic acid solution of 1mol/L and the MgSO of 1mol/L
4Solution is precipitated after the stirring in a large number.
4, precipitation is carried out decompress filter, and repeatedly wash filter residue with hot water, flush away emulsifying agent wherein filters, and after the oven dry, pulverizes, and obtains monomer conversion and be 92.2% anti-dripping agent.
Claims (4)
1. the anti-dripping agent preparation method based on the electrostatic adhesion parcel is characterized in that its preparation method is: after 1, certain two kinds of reaction monomers being measured according to 4: 1 ratio, add 1% cats product, carry out pre-emulsification, obtain pre-emulsion; 2, pre-emulsion is added in the round-bottomed flask, add the deionized water that is about 2 times of monomer total amounts, after mixing, keep rotating speed 120r/min, carried out polyreaction 6-8 hour at 70-80 ℃, be cooled to room temperature after reaction finishes and obtain polymer emulsion; 3, the partial polymer emulsion is added in the polytetrafluoroethyldispersion dispersion of equivalent, precipitated in a large number after the heated and stirred; 4, precipitation is carried out decompress filter, with certain method flush away emulsifying agent wherein, oven dry is pulverized, and obtains described anti-dripping agent.
2. a kind of anti-dripping agent preparation method based on electrostatic adhesion parcel according to claim 1 is characterized in that described polymer monomer is one of following or wherein two or more mixing: methyl methacrylate, vinylbenzene, divinyl, butyl methacrylate, vinyl cyanide, methacrylic acid.
3. a kind of anti-dripping agent preparation method based on electrostatic adhesion parcel according to claim 1 is characterized in that described cats product is one of following or wherein two or more mixing: dodecyl benzyl dimethyl ammonium chloride, palmityl trimethyl ammonium chloride, cetyl trimethylammonium bromide, octadecyl trimethyl ammonium chloride.
4. a kind of anti-dripping agent preparation method based on electrostatic adhesion parcel according to claim 1 is characterized in that described initiator is one of following or wherein two or more mixing: Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile), benzoyl peroxide, Potassium Persulphate, ammonium persulphate.
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| CN 201210123799 CN103374136A (en) | 2012-04-20 | 2012-04-20 | Preparation method of anti-drip agent based on electrostatic adsorption and wrapping |
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| CN 201210123799 CN103374136A (en) | 2012-04-20 | 2012-04-20 | Preparation method of anti-drip agent based on electrostatic adsorption and wrapping |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103665236A (en) * | 2013-12-18 | 2014-03-26 | 常熟振氟新材料有限公司 | Preparation method of anti-dripping agent |
| CN106947035A (en) * | 2017-04-10 | 2017-07-14 | 广东优科艾迪高分子材料有限公司 | A kind of anti-dripping melt type organic sesqui siloxane fire retardant and preparation method and application |
| CN110540613A (en) * | 2019-09-23 | 2019-12-06 | 铨盛聚碳科技股份有限公司 | anti-dripping macromolecular sulfonate flame retardant and preparation method thereof |
-
2012
- 2012-04-20 CN CN 201210123799 patent/CN103374136A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103665236A (en) * | 2013-12-18 | 2014-03-26 | 常熟振氟新材料有限公司 | Preparation method of anti-dripping agent |
| CN106947035A (en) * | 2017-04-10 | 2017-07-14 | 广东优科艾迪高分子材料有限公司 | A kind of anti-dripping melt type organic sesqui siloxane fire retardant and preparation method and application |
| CN110540613A (en) * | 2019-09-23 | 2019-12-06 | 铨盛聚碳科技股份有限公司 | anti-dripping macromolecular sulfonate flame retardant and preparation method thereof |
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Application publication date: 20131030 |