CN102432732B - Preparation method for polyvinyl chloride resin used for flame-retardant cable - Google Patents
Preparation method for polyvinyl chloride resin used for flame-retardant cable Download PDFInfo
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- CN102432732B CN102432732B CN201110069731.8A CN201110069731A CN102432732B CN 102432732 B CN102432732 B CN 102432732B CN 201110069731 A CN201110069731 A CN 201110069731A CN 102432732 B CN102432732 B CN 102432732B
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Abstract
The invention relates to a formula and a production technology of polyvinyl chloride resin used for a flame-retardant cable. A suspending polymerization method is adopted and comprises the following steps: adding a vinyl chloride monomer, a stabilizing agent, a dispersing agent, a novel fire retardant, a chain extender, auxiliaries and de-ionized water into a polymerization kettle; cold stirring for 30 minutes; reacting for 5-6.5 hours at 50-60 DEG C; and after reducing pressure for 0.1 MPa, adding a terminator, thereby obtaining a water suspending solution of the polyvinyl chloride resin for the flame-retardant cable. The unreacted vinyl chloride monomer is removed, and centrifugal drying is performed, thereby obtaining an end product. The polyvinyl chloride resin used for the flame-retardant cable produced according to the production technology has the advantages that the form of grains in the product is regular, the plasticizing property is excellent, the mobility of flux is high, the additional fire retardant is unnecessary in the formula of the product, and the flame retardation of a material is obviously promoted. The product is mainly applied to the material with high demand on flame retardation, such as electric wires and cables, and the like.
Description
Technical field:
The present invention relates to a kind of preparation method of polyvinyl chloride (PVC) RESINS, relate in particular to a kind of preparation method who is applied to the polyvinyl chloride (PVC) RESINS of producing flame retardant cable.
Background technology:
The features such as insulation layer and sheath require material mechanical good physical performance for electric wire, electrical property is good, flame retardant properties good, possess photostabilization, chemical proofing, winter hardiness, oil-proofness, especially propose certain requirement to snappiness.The universal polyvinyl chloride (PVC) RESINS molecular weight that processing cable material uses is at present large, plasticization temperature is had relatively high expectations, extrude in processing Resin Flow poor, so in the course of processing of cable sheath, general employing various functional agent physical mixed such as universal resin and softening agent, fire retardants, by high-speed kneading, low speed coldly stir, extruding pelletization operation, finally utilize pellet as the production technique of producing wire cable insulating layer or sheath.Therefore exist fire retardant to disperse in polyvinyl chloride (PVC) RESINS uneven, reduced mechanical property and the flame retardant properties of polyvinyl chloride cable material.Along with Domestic Scientific Research strength is strengthened, the technological improvement of the factors such as the exploitation of polyvinyl chloride functional agent used, production technique, equipment, the flame retardant properties of flame retardant cable polyvinyl chloride improves, but can't meet the application on high flame resistance product.
Summary of the invention:
The technical problem to be solved in the present invention is to provide a kind of preparation method of polyvinyl chloride resin used for flame-retardant cable, improves the flame retardant properties of cable pvc material.
In order to solve the problems of the technologies described above, the present invention realizes by following steps:
(1) first molybdic oxide, aluminium hydroxide, magnesium hydroxide are mixed according to the ratio of 1: 15: 5, add again deionized water to mix and be made into suspension with anion surfactant, with pH=4.5～6.5 of hydrochloric acid regulation system, at 75～80 DEG C, stir 4～6h, then filter washing, and be dried to constant weight at 50 DEG C, and making composite flame-retardant agent, the add-on of composite flame-retardant agent in polymerization is 1%～8%;
(2) by vinyl chloride monomer, stablizer, dispersion agent, composite flame-retardant agent, chainextender, auxiliary agent and deionized water are added in polymeric kettle, cold stirring 30 minutes, at the temperature of 50-60 DEG C, reaction 5-6.5 hour, after step-down 0.1MPa, add terminator, obtain the aqeous suspension of polyvinyl chloride resin used for flame-retardant cable, by removing unreacted vinyl chloride monomer, centrifugal drying obtains finished product.
Described anion surfactant is sodium lauryl sulphate, Sodium palmityl sulfate, Sodium dodecylbenzene sulfonate or hexadecyl benzene sulfonic acid sodium salt, and add-on is that anion surfactant and flame-retardant mixture mass ratio are 0.1～0.5.
Described initiator comprise peroxidation neodecanoic acid isopropyl phenyl ester, peroxy dicarbonate ethylhexyl, new peroxide tert-butyl caprate or peroxidation neodecanoic acid front three pentyl ester one or more, in polymerization, add-on is 0.4%-0.7%.
Described dispersion agent be high alcoholysis degree polyvinyl alcohol (alcoholysis degree >=80%), middle alcoholysis degree polyvinyl alcohol (alcoholysis degree 60%-70%), polyvinyl alcohol with low alcoholysis level (alcoholysis degree≤50%) or Vltra tears one or more, the add-on in polymerization is 0.3%-0.8%.
Described chainextender be triallyl cyanurate, diallyl maleate, adjacent benzoic acid diallyl one or more, the add-on in polymerization is 0.05-0.1%.
Other reaction conditions of the present invention is identical with conventional production process of resin with resin slurry aftertreatment technology, and polymeric reaction temperature is 50-60 DEG C, and the reaction times is 300～360min.
Advantage of the present invention is fairly obvious, and the product polyvinyl chloride resin used for flame-retardant cable of manufacturing of the present invention adopts suspension polymerization to produce, and before beginning polymerization, chainextender is mixed with vinyl chloride monomer, then adds polymerization in still.In reaction, chainextender connects skill to polyvinyl chloride macro-radical, and grafted chain is extended, and makes resin have better heat-resisting, resistance to solvent, physical strength and finish size stability; In polymerization, add fire retardant to react with vinyl chloride monomer, in reaction, vinylchlorid macromole connects skill and carries out polymerization to fire retardant surface, has improved the dispersing property of fire retardant in resin, makes resin have better flame retardant properties.This product is in the course of processing of cable sheath, and compared with ordinary resin processing cable sheath, product particle form is regular, and plasticizing capacity is good, makes polyvinyl chloride (PVC) RESINS fluidity of molten high, has significantly improved forcing machine production efficiency.Meanwhile, do not need additionally to add fire retardant in goods formula, the flame retardant properties of the more universal resin of electric wire polyvinyl chloride insulation layer flame retardant properties is significantly improved.
Specific embodiments:
Below in conjunction with embodiment, the present invention is described in further detail:
Embodiment 1
By deionized water 14kg, vinyl chloride monomer 5kg, peroxidation neodecanoic acid isopropyl phenyl ester and peroxy dicarbonate ethylhexyl 5g, high alcoholysis degree polyvinyl alcohol/Vltra tears/polyvinyl alcohol with low alcoholysis level tri compound dispersion agent 7g, stablizer organotin and liquid zinc 2.73g, BACN 250g, bicarbonate of ammonia 3.52g, chainextender triallyl cyanurate 4.5g and 8.7gEDTA add in polymeric kettle, cold stirring after 30min under room temperature, be warming up to 58 ± 0.5 DEG C of polymerizations, react 6 hours, after step-down 0.1MPa, add terminator to finish polymerization, obtain the aqeous suspension of polyvinyl chloride resin used for flame-retardant cable.
Remove unreacted monomer, discharging, filters, the dry polyvinyl chloride resin used for flame-retardant cable that obtains.
Resin viscosity number is 138, and apparent density is 0.54g/ml, plasticizer absorption rate 28g/100g, and sieving rate (65 order/250 orders, %) is 98.2/1.4, whiteness 88, by the oxygen index 36 after the processing of cable sheath working method.
Embodiment 2
By deionized water 14kg, vinyl chloride monomer 5kg, peroxidation neodecanoic acid isopropyl phenyl ester and peroxy dicarbonate ethylhexyl 5g, high alcoholysis degree polyvinyl alcohol/middle alcoholysis degree polyvinyl alcohol/polyvinyl alcohol with low alcoholysis level tri compound dispersion agent 7g, stablizer organotin and liquid zinc 2.73g, BACN 250g, bicarbonate of ammonia 3.52g, chainextender triallyl cyanurate 4.5g and 8.7gEDTA add in polymeric kettle, cold stirring after 30min under room temperature, be warming up to 58 ± 0.5 DEG C of polymerizations, react 6 hours, after step-down 0.1MPa, add terminator to finish polymerization, obtain the aqeous suspension of polyvinyl chloride resin used for flame-retardant cable.
Remove unreacted monomer, discharging, filters, the dry polyvinyl chloride resin used for flame-retardant cable that obtains.
Resin viscosity number is 138, and apparent density is 0.52g/ml, plasticizer absorption rate 28g/100g, and sieving rate (65 order/250 orders, %) is 97.2/1.0, whiteness 87, by the oxygen index 36 after the processing of cable sheath working method.
Embodiment 3
By deionized water 14kg, vinyl chloride monomer 5kg, peroxidation neodecanoic acid isopropyl phenyl ester and peroxy dicarbonate ethylhexyl 5g, high alcoholysis degree polyvinyl alcohol/Vltra tears/polyvinyl alcohol with low alcoholysis level tri compound dispersion agent 5g, stablizer organotin and liquid zinc 2.73g, BACN 250g, bicarbonate of ammonia 3.52g, chainextender triallyl cyanurate 4.5g and 8.7gEDTA add in polymeric kettle, cold stirring after 30min under room temperature, be warming up to 58 ± 0.5 DEG C of polymerizations, react 6 hours, after step-down 0.1MPa, add terminator to finish polymerization, obtain the aqeous suspension of polyvinyl chloride resin used for flame-retardant cable.
Remove unreacted monomer, discharging, filters, the dry polyvinyl chloride resin used for flame-retardant cable that obtains.
Resin viscosity number is 138, and apparent density is 0.52g/ml, plasticizer absorption rate 26g/100g, and sieving rate (65 order/250 orders, %) is 95.2/1.3, whiteness 87, by the oxygen index 35 after the processing of cable sheath working method.
Embodiment 4
By deionized water 14kg, vinyl chloride monomer 5kg, peroxidation neodecanoic acid isopropyl phenyl ester and peroxidation neodecanoic acid front three pentyl ester 5g, high alcoholysis degree polyvinyl alcohol/Vltra tears/polyvinyl alcohol with low alcoholysis level tri compound dispersion agent 7g, stablizer organotin and liquid zinc 2.73g, BACN 250g, bicarbonate of ammonia 3.52g, chainextender triallyl cyanurate 4.5g and 8.7gEDTA add in polymeric kettle, cold stirring after 30min under room temperature, be warming up to 58 ± 0.5 DEG C of polymerizations, react 6.5 hours, after step-down 0.1MPa, add terminator to finish polymerization, obtain the aqeous suspension of polyvinyl chloride resin used for flame-retardant cable.
Remove unreacted monomer, discharging, filters, the dry polyvinyl chloride resin used for flame-retardant cable that obtains.
Resin viscosity number is 138, and apparent density is 0.53g/ml, plasticizer absorption rate 28g/100g, and sieving rate (65 order/250 orders, %) is 98.5/1.1, whiteness 88, by the oxygen index 36 after the processing of cable sheath working method.
Embodiment 5
By deionized water 14kg, vinyl chloride monomer 5kg, peroxidation neodecanoic acid isopropyl phenyl ester and peroxy dicarbonate ethylhexyl 6g, high alcoholysis degree polyvinyl alcohol/Vltra tears/polyvinyl alcohol with low alcoholysis level tri compound dispersion agent 7g, stablizer organotin and liquid zinc 2.73g, BACN 250g, bicarbonate of ammonia 3.52g, chainextender triallyl cyanurate 4.5g and 8.7gEDTA add in polymeric kettle, cold stirring after 30min under room temperature, be warming up to 58 ± 0.5 DEG C of polymerizations, react 5.5 hours, after step-down 0.1MPa, add terminator to finish polymerization, obtain the aqeous suspension of polyvinyl chloride resin used for flame-retardant cable.
Remove unreacted monomer, discharging, filters, the dry polyvinyl chloride resin used for flame-retardant cable that obtains.
Resin viscosity number is 139, and apparent density is 0.53g/ml, plasticizer absorption rate 27g/100g, and sieving rate (65 order/250 orders, %) is 97.3/1.5, whiteness 87, by the oxygen index 36 after the processing of cable sheath working method.
Embodiment 6
By deionized water 14kg, vinyl chloride monomer 5kg, peroxidation neodecanoic acid isopropyl phenyl ester and peroxy dicarbonate ethylhexyl 5g, high alcoholysis degree polyvinyl alcohol/Vltra tears/polyvinyl alcohol with low alcoholysis level tri compound dispersion agent 7g, stablizer organotin and liquid zinc 2.73g, BACN 300g, bicarbonate of ammonia 3.52g, chainextender triallyl cyanurate 4.5g and 8.7gEDTA add in polymeric kettle, cold stirring after 30min under room temperature, be warming up to 58 ± 0.5 DEG C of polymerizations, react 5.8 hours, after step-down 0.1MPa, add terminator to finish polymerization, obtain the aqeous suspension of polyvinyl chloride resin used for flame-retardant cable.
Remove unreacted monomer, discharging, filters, the dry polyvinyl chloride resin used for flame-retardant cable that obtains.
Resin viscosity number is 139, and apparent density is 0.54g/ml, plasticizer absorption rate 27g/100g, and sieving rate (65 order/250 orders, %) is 97.9/0.6, whiteness 87, by the oxygen index 37 after the processing of cable sheath working method.
Embodiment 7
By deionized water 14kg, vinyl chloride monomer 5kg, peroxidation neodecanoic acid isopropyl phenyl ester and peroxy dicarbonate ethylhexyl 5g, high alcoholysis degree polyvinyl alcohol/Vltra tears/polyvinyl alcohol with low alcoholysis level tri compound dispersion agent 7g, stablizer organotin and liquid zinc 2.73g, BACN 250g, bicarbonate of ammonia 3.52g, chainextender triallyl cyanurate 5g and 8.7gEDTA add in polymeric kettle, cold stirring after 30min under room temperature, be warming up to 58 ± 0.5 DEG C of polymerizations, react 6.2 hours, after step-down 0.1MPa, add terminator to finish polymerization, obtain the aqeous suspension of polyvinyl chloride resin used for flame-retardant cable.
Remove unreacted monomer, discharging, filters, the dry polyvinyl chloride resin used for flame-retardant cable that obtains.
Resin viscosity number is 140, and apparent density is 0.55g/ml, plasticizer absorption rate 28g/100g, and sieving rate (65 order/250 orders, %) is 97.2/0.7, whiteness 88, by the oxygen index 36 after the processing of cable sheath working method.
Embodiment 8
By deionized water 14kg, vinyl chloride monomer 5kg, peroxidation neodecanoic acid isopropyl phenyl ester and peroxy dicarbonate ethylhexyl 5g, high alcoholysis degree polyvinyl alcohol/Vltra tears/polyvinyl alcohol with low alcoholysis level tri compound dispersion agent 7g, stablizer organotin and liquid zinc 2.73g, BACN 250g, bicarbonate of ammonia 3.52g, chainextender triallyl cyanurate and diallyl maleate 5g and 8.7gEDTA add in polymeric kettle, cold stirring after 30min under room temperature, be warming up to 58 ± 0.5 DEG C of polymerizations, react 6.2 hours, after step-down 0.1MPa, add terminator to finish polymerization, obtain the aqeous suspension of polyvinyl chloride resin used for flame-retardant cable.
Remove unreacted monomer, discharging, filters, the dry polyvinyl chloride resin used for flame-retardant cable that obtains.
Resin viscosity number is 142, and apparent density is 0.54g/ml, plasticizer absorption rate 27g/100g, and sieving rate (65 order/250 orders, %) is 98.2/0.5, whiteness 88, by the oxygen index 36 after the processing of cable sheath working method.
By relatively can finding out of above 8 embodiment and comparative example, in polymerization reaction system, add different dispersion agent kind and consumption, sieving of resin particle is distributed with variation, apparent density also has corresponding variation, and best dispersant system is high alcoholysis degree polyvinyl alcohol/Vltra tears/polyvinyl alcohol with low alcoholysis level tri compound dispersant system.In polymerization reaction system, add different initiator kind and consumption, affected the reaction times of polymerization system, little on other impact.In polymerization reaction system, add different amount of flame-retardant agents, affected the oxygen index of resin, the increase of amount of flame-retardant agent, oxygen index is corresponding raising also.In polymerization reaction system, add different chainextender kind and consumption, the molecular weight of resin increases to some extent.
Claims (2)
1. a preparation method for polyvinyl chloride resin used for flame-retardant cable, is characterized in that, the step of method is:
1) first molybdic oxide, aluminium hydroxide, magnesium hydroxide are mixed according to the ratio of 1: 15: 5, add again deionized water to mix and be made into suspension with anion surfactant, with pH=4.5～6.5 of hydrochloric acid regulation system, at 75～80 DEG C, stir 4～6h, then filter washing, and be dried to constant weight at 50 DEG C, and making composite flame-retardant agent, the add-on of composite flame-retardant agent in polymerization is 1%～8%;
2) by vinyl chloride monomer, stablizer, dispersion agent, composite flame-retardant agent, chainextender, auxiliary agent and deionized water are added in polymeric kettle, cold stirring 30 minutes, at the temperature of 50-60 DEG C, reaction 5-6.5 hour, after step-down 0.1MPa, add terminator, obtain the aqeous suspension of polyvinyl chloride resin used for flame-retardant cable, by removing unreacted vinyl chloride monomer, centrifugal drying obtains finished product.
2. the preparation method of a kind of polyvinyl chloride resin used for flame-retardant cable according to claim 1, it is characterized in that the preparation of composite flame-retardant agent, employing anion surfactant is sodium lauryl sulphate, Sodium palmityl sulfate, Sodium dodecylbenzene sulfonate or hexadecyl benzene sulfonic acid sodium salt, and add-on is that anion surfactant and flame-retardant mixture mass ratio are 0.1～0.5.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103289003B (en) * | 2013-05-23 | 2016-03-09 | 吴江市风尚鞋厂 | A kind of HPVC resin material and preparation method thereof |
| CN107492412A (en) * | 2016-05-26 | 2017-12-19 | 石策略 | A kind of Anti-interference cable |
| CN106749797B (en) * | 2016-12-14 | 2019-03-05 | 青海盐湖工业股份有限公司 | A kind of preparation method of polyvinyl chloride |
| CN108659409B (en) * | 2018-06-21 | 2020-12-15 | 江苏新汇烽塑胶有限公司 | High-temperature-resistant polyvinyl chloride resin and preparation method thereof |
| CN114478883A (en) * | 2020-10-28 | 2022-05-13 | 中国石油化工股份有限公司 | Preparation method of high-porosity low-involucra HPVC resin |
| CN116510654A (en) * | 2023-03-13 | 2023-08-01 | 苏州汇博塑化有限公司 | Polyvinyl chloride flame-retardant elastomer insulating material preparation device and preparation method thereof |
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Effective date of registration: 20190328 Address after: No. 36 North Sandong Road, Shihezi Economic and Technological Development Zone, Xinjiang, 832000 Patentee after: Xinjiang Tianye (Group) Co., Ltd. Address before: 832000 Xinjiang Uygur Autonomous Region Shihezi West Third Road North End of China Chemical Co., Ltd. Patentee before: Shihezi Zhongfa Chemical Co., Ltd., Xinjiang |