CN105331039A - Preparation method of modified resin - Google Patents
Preparation method of modified resin Download PDFInfo
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- CN105331039A CN105331039A CN201510780472.8A CN201510780472A CN105331039A CN 105331039 A CN105331039 A CN 105331039A CN 201510780472 A CN201510780472 A CN 201510780472A CN 105331039 A CN105331039 A CN 105331039A
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Abstract
The invention provides a preparation method of modified resin. The method comprises the steps that 80-100 parts of ABS fine particles, 80-100 parts of resin particles, 25 parts of talcum powder, 0.5 part of isopropyl tri(dioctylpyrophosphate) titanate, 0.1 part of lubricant stearic acid and 0.2 part of antioxygen are added into a high-speed mixer, mixing is conducted for 5 min, the mixture is added into a twin-screw extruder from a feed inlet of an extruder, the extrusion temperatures are 200 DEG C, 235 DEG C, 240 DEG C, 240 DEG C and 245 DEG C respectively, extruding and granulating are conducted, and the modified resin is obtained. The modified resin prepared through the method has the advantages of being good in high-temperature stability, flame retardant property and anti-adhering tin property.
Description
Technical field
The invention belongs to technical field of macromolecules, be specifically related to a kind of preparation method of modified resin.
Background technology
Acrylonitrile-butadiene-styrene copolymer resin (ABS), there is the comprehensive physical property that high impact, high heat-resisting and low temperature resistant, resistance to chemical attack, electrical insulation capability etc. are excellent, and having excellent processing characteristics, plating performance and high gloss outward appearance, is that consumption is maximum, purposes one of engineering plastics the most widely.
But ABS resin oxygen index is only 18.3-20, belonging to inflammable macromolecular material, when products such as the various electronic apparatuss for having flame-retardancy requirements, needing to carry out flame-retardant modified, to meet the service requirements of fire safety.The most ripe at present, the most effective ABS method for modifying flame adds bromide fire retardant, the V0 level of shiploads of merchandise, V2 level flame-proof ABS has been widely used in the fields such as electronics, Communication Equipment, automotive industry, household electrical appliance, office equipment, electric product.
At present, when flame-proof ABS is applied in electrical and electronic component, often need to carry out circuit card soldering.But there is the problem of easily sticky tin when crossing tin bath in flame-proof ABS product, this be due to:
(1) although the time crossing tin bath is shorter, 10-30s, tin bath temperatures as high 250-350 DEG C, the texturing temperature of the flame-proof ABS of itself is only about 80 DEG C, so easily cause the distortion of product, adds the contact area of product and tin bath.
(2) heat decomposition temperature of fire retardant is usually lower, very easily decomposes when 250-350 DEG C, and what exist in fire retardant in addition residually also easily volatilizees, and causes the uneven of article surface, adds the contact area of itself and tin bath.
(3) owing to the addition of bromide fire retardant, polarity is higher, and surface energy is larger, makes flame-proof ABS that sticky tin phenomenon more easily occur.
Existence due to sticky tin brings at follow-up and electric wire, causes the risk of short circuit during the electric elements such as semi-conductor use jointly, greatly threatens the safety of lives and properties, and this is definitely unallowed.Flame-proof ABS must ensure its anti-solder-adhering performance in electrification uses as can be seen here.
Summary of the invention
Goal of the invention: for the deficiencies in the prior art, the invention provides a kind of preparation method of modified resin.
Technical scheme: the preparation method that the invention provides a kind of modified resin: 80 ~ 100 parts of ABS fine particles and 80 ~ 100 parts of resin particles are added 25 parts of talcum powder, 0.5 part of sec.-propyl three (dioctyl phosphoric acid acyloxy) titanic acid ester, 0.1 part of lubricant stearic acid, 0.2 part of oxidation inhibitor adds in high-speed mixer, mix 5 minutes, compound is added twin screw extruder from forcing machine charging opening, extrusion temperature is respectively 200 DEG C, 235 DEG C, 240 DEG C, 240 DEG C, 245 DEG C, extruding pelletization, obtains modified resin.
Concrete, described oxidation inhibitor is the mixture of antioxidant 1076 and oxidation inhibitor 626, and both mass ratioes are 1:1.
Concrete, described resin particle obtains by the following method: the material that styrene monomer, vinyl cyanide and solvent ethylbenzene form is entered polymeric kettle after preheating, polymeric reaction temperature is 120 ~ 150 degrees Celsius, pressure 0.196 ~ 0.294 MPa, then after being heated to 240 DEG C, under 2.67 kpa pressures, remove the volatiless such as remaining styrene monomer again, obtain the resin of molten, after cooling, extrusion pelletizing obtains resin particle.
In above-mentioned steps, described vinyl cyanide: styrene monomer=30:70, ethylbenzene accounts for 5% ~ 10% of monomer weight.
: after polymerization remove most of vinyl cyanide and portion of styrene monomer, ethylbenzene volatiles by from polymeric kettle material flash distillation under 0.196 MPa out, and then heat the further improvement of above-mentioned steps.
Concrete, the fine grain preparation method of described ABS is: by polybutadiene latex obtained above 5 ~ 15 parts, third rare nitrile 15 ~ 40 parts, styrene monomer 60 ~ 85 parts joins in reactor, take dicumyl peroxide as initiator, temperature of reaction is 90 DEG C, 5 hours reaction times, condense after reaction terminates, flocculation agent is dilute sulphuric acid or alum, condensation temperature 90 DEG C, after cohesion after washing, drying, the ABS fine particle obtained.
The preparation method of the polybutadiene latex described in above-mentioned steps is: add in polymeric kettle by the compounding agent solution of emulsifying agent oleic acid potash soap 1 ~ 2 part, 5 ~ 15 parts, mercaptan, Potassium Persulphate 0.5 ~ 1 part composition together with divinyl 100 parts, temperature of reaction 90 ~ 93 DEG C, 16 hours reaction times, after reaction, with liquefied ammonia cooling, obtain polybutadiene latex.
Beneficial effect: adopt the modified resin that the method for the invention is obtained, there is good high-temperature stability, good flame retardant properties and anti-solder-adhering performance.
Embodiment:
Embodiment 1
The compounding agent solution of emulsifying agent oleic acid potash soap 1g, mercaptan 5g, Potassium Persulphate 0.5g composition is added in polymeric kettle together with divinyl 100g, temperature of reaction 90 DEG C, 16 hours reaction times, after reaction, with liquefied ammonia cooling, obtain polybutadiene latex.
By polybutadiene latex 5g obtained above, third rare nitrile 15g, styrene monomer 60g joins in reactor, take dicumyl peroxide as initiator, temperature of reaction is 90 DEG C, in 5 hours reaction times, condense after reaction terminates, flocculation agent is dilute sulphuric acid or alum, condensation temperature 90 DEG C, after condensing the ABS fine particle washing obtained, dry, for subsequent use.
The material be made up of styrene monomer, vinyl cyanide and solvent ethylbenzene enters polymeric kettle, vinyl cyanide after preheating: styrene monomer=30:70, and ethylbenzene accounts for 5% of monomer weight.Polymeric reaction temperature is 120 degrees Celsius, pressure 0.196 MPa, removes most of vinyl cyanide and the volatiles such as portion of styrene monomer, ethylbenzene after reaction from polymeric kettle material flash distillation under 0.196 MPa out.Then after being heated to 240 degrees Celsius, removing the volatiless such as remaining styrene monomer again, obtain the resin of molten under 2.67 kpa pressures, after cooling, extrusion pelletizing obtains resin particle.
100gABS fine particle and 100g resin particle are added 25g talcum powder, 0.5g sec.-propyl three (dioctyl phosphoric acid acyloxy) titanic acid ester, 0.1g lubricant stearic acid, 0.1g antioxidant 1076 and 0.1g oxidation inhibitor 626 add in high-speed mixer, mix 5 minutes.Compound is added twin screw extruder from forcing machine charging opening, and extrusion temperature is respectively 200 DEG C, 235 DEG C, 240 DEG C, 240 DEG C, 245 DEG C, extruding pelletization.
Embodiment 2
The compounding agent solution of emulsifying agent oleic acid potash soap 2g, mercaptan 15g, Potassium Persulphate 1g composition is added in polymeric kettle together with divinyl 100g, temperature of reaction 93 DEG C, 16 hours reaction times, after reaction, with liquefied ammonia cooling, obtain polybutadiene latex.
By polybutadiene latex 15g obtained above, third rare nitrile 40g, styrene monomer 85g joins in reactor, take dicumyl peroxide as initiator, temperature of reaction is 90 DEG C, in 5 hours reaction times, condense after reaction terminates, flocculation agent is dilute sulphuric acid or alum, condensation temperature 90 DEG C, after condensing the ABS fine particle washing obtained, dry, for subsequent use.
The material be made up of styrene monomer, vinyl cyanide and solvent ethylbenzene enters polymeric kettle, vinyl cyanide after preheating: styrene monomer=30:70, and ethylbenzene accounts for 10% of monomer weight.Polymeric reaction temperature is 150 degrees Celsius, pressure 0.294 MPa, removes most of vinyl cyanide and the volatiles such as portion of styrene monomer, ethylbenzene after reaction from polymeric kettle material flash distillation under 0.196 MPa out.Then after being heated to 240 degrees Celsius, removing the volatiless such as remaining styrene monomer again, obtain the resin of molten under 2.67 kpa pressures, after cooling, extrusion pelletizing obtains resin particle.
100gABS fine particle and 100g resin particle are added 25g talcum powder, 0.5g sec.-propyl three (dioctyl phosphoric acid acyloxy) titanic acid ester, 0.1g lubricant stearic acid, 0.1g antioxidant 1076 and 0.1g oxidation inhibitor 626 add in high-speed mixer, mix 5 minutes.Compound is added twin screw extruder from forcing machine charging opening, and extrusion temperature is respectively 200 DEG C, 235 DEG C, 240 DEG C, 240 DEG C, 245 DEG C, extruding pelletization.
Embodiment 3
The compounding agent solution of emulsifying agent oleic acid potash soap 1g, mercaptan 15g, Potassium Persulphate 0.5g composition is added in polymeric kettle together with divinyl 100g, temperature of reaction 90 ~ 93 DEG C, 16 hours reaction times, after reaction, with liquefied ammonia cooling, obtain polybutadiene latex.
By polybutadiene latex 15g obtained above, third rare nitrile 15g, styrene monomer 85g joins in reactor, take dicumyl peroxide as initiator, temperature of reaction is 90 DEG C, in 5 hours reaction times, condense after reaction terminates, flocculation agent is dilute sulphuric acid or alum, condensation temperature 90 DEG C, after condensing the ABS fine particle washing obtained, dry, for subsequent use.
The material be made up of styrene monomer, vinyl cyanide and solvent ethylbenzene enters polymeric kettle, vinyl cyanide after preheating: styrene monomer=30:70, and ethylbenzene accounts for 5%% of monomer weight.Polymeric reaction temperature is 150 degrees Celsius, pressure 0.294 MPa, removes most of vinyl cyanide and the volatiles such as portion of styrene monomer, ethylbenzene after reaction from polymeric kettle material flash distillation under 0.196 MPa out.Then after being heated to 240 degrees Celsius, removing the volatiless such as remaining styrene monomer again, obtain the resin of molten under 2.67 kpa pressures, after cooling, extrusion pelletizing obtains resin particle.
100gABS fine particle and 100g resin particle are added 25g talcum powder, 0.5g sec.-propyl three (dioctyl phosphoric acid acyloxy) titanic acid ester, 0.1g lubricant stearic acid, 0.1g antioxidant 1076 and 0.1g oxidation inhibitor 626 add in high-speed mixer, mix 5 minutes.Compound is added twin screw extruder from forcing machine charging opening, and extrusion temperature is respectively 200 DEG C, 235 DEG C, 240 DEG C, 240 DEG C, 245 DEG C, extruding pelletization.
Embodiment 4
The compounding agent solution of emulsifying agent oleic acid potash soap 1g, mercaptan 5g, Potassium Persulphate 1g composition is added in polymeric kettle together with divinyl 100g, temperature of reaction 90 DEG C, 16 hours reaction times, after reaction, with liquefied ammonia cooling, obtain polybutadiene latex.
By polybutadiene latex 15g obtained above, third rare nitrile 40g, styrene monomer 85g joins in reactor, take dicumyl peroxide as initiator, temperature of reaction is 90 DEG C, in 5 hours reaction times, condense after reaction terminates, flocculation agent is dilute sulphuric acid or alum, condensation temperature 90 DEG C, after condensing the ABS fine particle washing obtained, dry, for subsequent use.
The material be made up of styrene monomer, vinyl cyanide and solvent ethylbenzene enters polymeric kettle, vinyl cyanide after preheating: styrene monomer=30:70, and ethylbenzene accounts for 5% of monomer weight.Polymeric reaction temperature is 150 degrees Celsius, pressure 0.294 MPa, removes most of vinyl cyanide and the volatiles such as portion of styrene monomer, ethylbenzene after reaction from polymeric kettle material flash distillation under 0.196 MPa out.Then after being heated to 240 degrees Celsius, removing the volatiless such as remaining styrene monomer again, obtain the resin of molten under 2.67 kpa pressures, after cooling, extrusion pelletizing obtains resin particle.
100gABS fine particle and 100g resin particle are added 25g talcum powder, 0.5g sec.-propyl three (dioctyl phosphoric acid acyloxy) titanic acid ester, 0.1g lubricant stearic acid, 0.1g antioxidant 1076 and 0.1g oxidation inhibitor 626 add in high-speed mixer, mix 5 minutes.Compound is added twin screw extruder from forcing machine charging opening, and extrusion temperature is respectively 200 DEG C, 235 DEG C, 240 DEG C, 240 DEG C, 245 DEG C, extruding pelletization.
By modified resin that the various embodiments described above obtain, insert the liquid tin bath of 250 DEG C, soak 10S, then pull out from tin bath with constant speed, test according to GB/T2918-1998 standard.In addition, high temperature resistant test is carried out to the modified resin of the various embodiments described above gained.The results are shown in following table.
| Anti-solder-adhering ability | 250 DEG C of high temperature resistant tests | 400 DEG C of high temperature resistant tests | |
| Embodiment 1 | Average tin sweat(ing) number 1/cm 2 | Undeformed | Undeformed |
| Embodiment 2 | Average tin sweat(ing) number 2/cm 2 | Undeformed | Undeformed |
| Embodiment 3 | Average tin sweat(ing) number 1/cm 2 | Undeformed | Undeformed |
| Embodiment 4 | Average tin sweat(ing) number 1/cm 2 | Undeformed | Undeformed |
| Ordinary resin | Average tin sweat(ing) number 4/cm 2 | Undeformed | Curling, surperficial deliquescing |
Claims (7)
1. the preparation method of a modified resin, 80 ~ 100 parts of ABS fine particles and 80 ~ 100 parts of resin particles are it is characterized in that to add 25 parts of talcum powder, 0.5 part of sec.-propyl three (dioctyl phosphoric acid acyloxy) titanic acid ester, 0.1 part of lubricant stearic acid, 0.2 part of oxidation inhibitor adds in high-speed mixer, mix 5 minutes, compound is added twin screw extruder from forcing machine charging opening, extrusion temperature is respectively 200 DEG C, 235 DEG C, 240 DEG C, 240 DEG C, 245 DEG C, extruding pelletization, obtains modified resin.
2. the preparation method of modified resin as claimed in claim 1, it is characterized in that described oxidation inhibitor is the mixture of antioxidant 1076 and oxidation inhibitor 626, both mass ratioes are 1:1.
3. the preparation method of modified resin as claimed in claim 1, it is characterized in that described resin particle obtains by the following method: the material that styrene monomer, vinyl cyanide and solvent ethylbenzene form is entered polymeric kettle after preheating, polymeric reaction temperature is 120 ~ 150 degrees Celsius, pressure 0.196 ~ 0.294 MPa, then after being heated to 240 DEG C, the volatiless such as remaining styrene monomer are removed again under 2.67 kpa pressures, obtain the resin of molten, after cooling, extrusion pelletizing obtains resin particle.
4. the preparation method of modified resin as claimed in claim 3, it is characterized in that described vinyl cyanide: styrene monomer=30:70, ethylbenzene accounts for 5% ~ 10% of monomer weight.
5. the preparation method of modified resin as claimed in claim 3, removes most of vinyl cyanide and portion of styrene monomer, ethylbenzene volatiles from polymeric kettle material flash distillation under 0.196 MPa out after it is characterized in that polyreaction, and then heats.
6. the preparation method of modified resin as claimed in claim 1, is characterized in that the fine grain preparation method of described ABS is: by polybutadiene latex obtained above 5 ~ 15 parts, third rare nitrile 15 ~ 40 parts, styrene monomer 60 ~ 85 parts joins in reactor, take dicumyl peroxide as initiator, temperature of reaction is 90 DEG C, 5 hours reaction times, condense after reaction terminates, flocculation agent is dilute sulphuric acid or alum, condensation temperature 90 DEG C, after cohesion after washing, drying, the ABS fine particle obtained.
7. the preparation method of modified resin as claimed in claim 6, it is characterized in that the preparation method of described polybutadiene latex is: add in polymeric kettle by the compounding agent solution of emulsifying agent oleic acid potash soap 1 ~ 2 part, 5 ~ 15 parts, mercaptan, Potassium Persulphate 0.5 ~ 1 part composition together with divinyl 100 parts, temperature of reaction 90 ~ 93 DEG C, 16 hours reaction times, after reaction, with liquefied ammonia cooling, obtain polybutadiene latex.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510780472.8A CN105331039A (en) | 2015-11-13 | 2015-11-13 | Preparation method of modified resin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510780472.8A CN105331039A (en) | 2015-11-13 | 2015-11-13 | Preparation method of modified resin |
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| CN105331039A true CN105331039A (en) | 2016-02-17 |
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| CN201510780472.8A Withdrawn CN105331039A (en) | 2015-11-13 | 2015-11-13 | Preparation method of modified resin |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109294153A (en) * | 2018-09-10 | 2019-02-01 | 浙江畅通科技有限公司 | A kind of anti-oxidant plastic housing of lead-acid accumulator and preparation method thereof |
| CN110406204A (en) * | 2019-07-29 | 2019-11-05 | 宁波速派电器有限公司 | A kind of modified Pa 6 material |
| CN113943470A (en) * | 2021-08-19 | 2022-01-18 | 创合新材料科技江苏有限公司 | High-temperature-resistant and non-deformable plastic ABS and preparation method thereof |
-
2015
- 2015-11-13 CN CN201510780472.8A patent/CN105331039A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109294153A (en) * | 2018-09-10 | 2019-02-01 | 浙江畅通科技有限公司 | A kind of anti-oxidant plastic housing of lead-acid accumulator and preparation method thereof |
| CN110406204A (en) * | 2019-07-29 | 2019-11-05 | 宁波速派电器有限公司 | A kind of modified Pa 6 material |
| CN113943470A (en) * | 2021-08-19 | 2022-01-18 | 创合新材料科技江苏有限公司 | High-temperature-resistant and non-deformable plastic ABS and preparation method thereof |
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Application publication date: 20160217 |