CN103554313A - Preparation method of chlorinated polyvinyl chloride for paint, coating and fiber - Google Patents
Preparation method of chlorinated polyvinyl chloride for paint, coating and fiber Download PDFInfo
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Abstract
The invention discloses a preparation method of chlorinated polyvinyl chloride for a paint, a coating and a fiber, and relates to the preparation method of the chlorinated polyvinyl chloride. The method comprises the following processes: dissolving an initiator into a solvent; dissolving polyvinyl chloride (PVC) into a solution, so as to form a PVC solution; vacuumizing and deoxidizing a reactor; introducing vaporized chlorine to chloridize; then blowing acid by nitrogen, so as to obtain chloridized liquid for water analysis; separating out the chloridized resin from a solvent phase by using hot water; preparing vinylidene chloride resin by dewatering and drying; separating out a solvent chlorobenzene from water by distillation of water vapor and recycling. By adopting the method, excellent PVC is taken as the raw material; the chlorobenzene is selected as the solvent; chlorination is carried out under the effects of the initiator and certain temperature, so as to obtain excellent vinylidene chloride resin for the paint, the coating and the fiber. By adopting special process technologies and conditions for acid blowing and chlorobenzene solvent recovery, the production capacity of the device is greatly increased; the investment and steam consumption are significantly reduced; the economic benefit is considerable.
Description
Technical field
The present invention relates to a kind of preparation method of chlorinated polyvinyl chloride, particularly relate to the preparation method of chlorinated polyvinyl chloride for a kind of paint, coating and fiber.
Background technology
Paint, coating and for fiber chlorinated polyvinyl chloride (also claiming supervinyi chloride resin) be by chlorination modified the making of polyvinyl chloride (PVC) resin, be a kind of paint of high-quality and the base-material of coating.This product is white or faint yellow tasteless, odorless, nontoxic loose particles or powder.PVC resin is after superchlorination, the irregularity that molecular chain is arranged increases, polarity increases, the solvability of resin is increased, under normal temperature, just can be dissolved in the organic solvents such as ketone, ester class, chlorinated hydrocarbon, nitro class, toluene, dimethylbenzene, under heating state, dissolve in benzene, aniline, phthalic acid dibutyl ester, tetracol phenixin etc.; Chemical stability increases, thereby has improved the performance of the corrosion of the thermotolerance of material and acid-and base-resisting, salt, oxygenant etc.Improved the mechanical property of the heat-drawn wire of resin, cl content is brought up to 61-65% by 56.7%, and vicat softening temperature is by 72-82 ℃, and (bringing up to 90-125 ℃), maximum operation (service) temperature can reach 110 ℃, and life-time service temperature is 95 ℃.
Supervinyi chloride resin can make multiple perchloropolyvinyl paint and coating.This kind of chlorinated polyvinyl chloride also can be made into chlorinated polyvinyl chloride fiber (being commonly called as chlorinated polyvinyl chloride fibre), and its fabric can be made the filter cloth of anti-chemical corrosion and special working suit, medical shirt etc., also can make the special filter cloth that atomic industry is used by direct spraying.Chlorinated polyvinyl chloride fiber also can be done ocean and use rope goods as fishing net, undersea cable crust etc.Can do the tackiness agent of plastics, rubber item and the non-blushing thinner in engineering, industrial putty etc.Because this chlorinated polyvinyl chloride has good electrical insulation capability, as insulating material, be widely used in electric utility.Chlorinated polyvinyl chloride can replace traditional thermoplastic engineering plastic, be widely used in the fields such as oil, chemical industry, building materials, shipbuilding, electrical equipment, printing and dyeing, plating, food and papermaking, mainly for the manufacture of heat-resisting, corrosion resistant pipeline and accessory, house pipe (hot water pipeline) system, communication pipeline system, blowdown pipelines etc.Meanwhile, according to the difference of chlorination degree, CPVC also can be used for modification, manufacture matrix material, foam material, coating and the tackiness agent etc. of chlorination fiber.In addition, CPVC also can be used as the properties-correcting agent of plastics, with thermoplasticity or thermosetting resin fusion blend alloying, improves the performance of material, makes it to become more superior engineering plastics.
The chlorinated polyvinyl chloride that only has solubilisate chloridization process to produce just can be applicable to paint and coating purposes, is also applicable to other purposes simultaneously.So-called solubilisate chloridization process is dissolved in PVC exactly and in certain solvent, forms PVC solution, then under the existence of initiator, pass into vaporization chlorine and carry out chlorination, then with nitrogen, blow acid and obtain conforming with the chlorated liquid that elutriation is used, water makes the resin after chlorination separate out from solvent phase, then through super-dry to make supervinyi chloride resin.Solvent recuperation is used again.The problem that existing solubilisate chloridization process exists has: material pvc, solvent are selected unreasonable, after first polyvinyl chloride, the dissolving order of initiator should change, normal pressure blows acid time length, consumption nitrogen amount is large, and solvent is reclaimed in air distillation, and steam consumption is high, the time is long etc.
Summary of the invention
The object of the present invention is to provide the preparation method of chlorinated polyvinyl chloride for a kind of paint, coating and fiber, the method employing PVC obtains paint, coating and fiber at Chlorine in Solution and with chlorinated polyvinyl chloride, also claims the method for supervinyi chloride resin, the method increases considerably the throughput of device, and investment and steam consumption significantly reduce.Economic benefit is very considerable.
The object of the invention is to be achieved through the following technical solutions:
The preparation method of chlorinated polyvinyl chloride for a kind of paint, coating and fiber, described method comprises following technique: initiator is dissolved in solvent, PVC is dissolved in and in above-mentioned solution, forms PVC solution, reactor is vacuumized to deoxidation, pass into vaporization chlorine and carry out chlorination, then with nitrogen, blow acid and obtain conforming with the chlorated liquid that elutriation is used, with hot water, the resin after chlorination is separated out from solvent phase, again through dehydration, the dry supervinyi chloride resin that makes, by wet distillation, from water, isolate solvent Benzene Chloride, recycling; The selected polyvinyl chloride resin polymerization degree should, at 850-950, preferably 900, be 22-30g/100g, preferably 24-28g/100g to plasticizer absorption; The polyvinyl chloride resin polymerization degree should, at 1350-1450, preferably 1400, be 26-34g/100g, preferably 28-32g/100g to plasticizer absorption; Solvent includes but not limited to tetracol phenixin, ethylene dichloride, tetrachloroethane and Benzene Chloride etc., the most handy Benzene Chloride, Benzene Chloride content>=99.2 W/%, polystream content≤0.65 W/%, moisture content≤5 * 10
-5massfraction; PVC chlorination initiator used includes but not limited to Diisopropyl azodicarboxylate, dilauroyl peroxide, and Diisopropyl azodicarboxylate is more conventional, first initiator is dissolved in Benzene Chloride, and then adds polyvinyl chloride resin; Operation is carried out under anoxybiotic state, and closed reactor is evacuated down to vacuum tightness 0.08Mpa, uses nitrogen vacuum breaker to normal pressure; Temperature of reaction is respectively 108 ± 0.3 ℃ and 112 ± 0.3 ℃, controls 5 ℃/min of heat-up rate <, and 3 ℃/min of < is better, preferably 2 ℃/min.Reaching 90-95 ℃ stops heating up; During 35 ℃ of reactor temperatures, start logical chlorine, logical chlorine speed is no more than 120 liters/h with per kilogram PVC and is advisable, be no more than 100 liters/h better, be preferably 90 liters/h. when reactor temperature reaches 85-90 ℃, increasing chlorine flux is no more than 240 liters/h with per kilogram PVC and is advisable, be no more than 200 liters/h better, optimum value is 150-170 liter/h; PVC chlorated liquid also will be used 0.5mpa(gauge pressure) nitrogen carries out vacuum and blows acid, at 0.1-0.001mpa, < 0.05mpa is better, preferably in 0.01mpa(absolute pressure) acid of pressure blowing down;
PVC Benzene Chloride solution also will carry out elutriation, and hot water (98-100 ℃) flow that enters Analytic Tower is chlorated liquid mass rate 50-100 times, and 70-90 is doubly better, preferably 80 times.
The preparation method of chlorinated polyvinyl chloride for described a kind of paint, coating and fiber, the 0.1-0.2(W/% that the consumption of described initiator is PVC).
The preparation method of chlorinated polyvinyl chloride for described a kind of paint, coating and fiber, the described Benzene Chloride stripping that also will reduce pressure reclaims, at 0.1-0.001mp, < 0.05mpa is better, preferably under 0.01mpa (absolute pressure) pressure, reclaims Benzene Chloride.
The preparation method of chlorinated polyvinyl chloride for described a kind of paint, coating and fiber, described stripping steam flow used should be chlorated liquid mass rate 0.7-2.5 times, 0.9-1.5 is doubly better, preferably 1 times, pressure 0.35-0.6mpa, is more preferably 0.4-0.5mpa, preferably 0.45mpa.
Advantage of the present invention and effect are:
The present invention be take the PVC of high-quality as raw material, and selective chlorination benzene is solvent, under initiator and certain temperature effect, carries out chlorination reaction, obtains the supervinyi chloride resin that paint, coating and the fiber of high-quality are used.Adopt special sour and Benzene Chloride solvent recovery process technology and the condition of blowing, the throughput of device increases considerably, and investment and steam consumption significantly reduce.Economic benefit is very considerable.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
The present invention be take the PVC of high-quality as raw material, selects suitable solvent, adopts special Technology and condition, obtains the supervinyi chloride resin of high-quality with lower consumption.
Available solvent includes but not limited to tetracol phenixin, ethylene dichloride, tetrachloroethane and Benzene Chloride etc., but wherein former three is low to polyvinyl chloride solubleness, and Chlorination speed is slow, and tetracol phenixin is the material of restricted use aspect environmental protection; When ethylene dichloride and tetrachloroethane are made solvent, also can there is chlorination reaction and generate many monochloroethane, make the recovery of solvent and reuse complicated.Only have Benzene Chloride (Benzene Chloride content > 99.2 W/%, W/% moisture content≤5 * 10, polystream content≤0.65
-5massfraction) the most applicable.The one, PVC solubleness in Benzene Chloride is larger, and the 2nd, the PVC chlorination reaction velocity being dissolved in Benzene Chloride is fast.The 3rd, chlorobenzene stability is high, does not react with this understanding, is conducive to recycling of solvent.
PVC is formed by chloroethylene polymerization, is by n-CH
2the macromole (-CH that-CHCl-unit forms
2-CHCl-) n, desirable chlorinated polyvinyl chloride should be every two-CH
2-CHCl-unit has a hydrogen atom to be replaced and form (-CHCl-CHCl-CH by chlorine
2-CHCl-CH
2-CHCl-) 1/3n structure, but be in fact far from being literally true, inhomogeneous chlorination is all greatly affected the chlorinated polyvinyl chloride obtaining in solubility property and result of use, therefore will try hard to make chlorination homogenizing as much as possible.Select specific polyvinyl chloride (PVC) RESINS.
The concentration of Benzene Chloride preparation polyvinyl chloride solution should be at 9-13.5(W/%).If solution is excessively rare, reaction is too fierce, easily causes chain rupture, makes low-molecular weight polymer too much.Also can produce excessive chlorination.Make plant factor reduce, the norm quota of consumption raises simultaneously; If strength of solution is too high, react inhomogeneous, finished product dissolves in bad order, and the chlorination reaction time is long, does not slowly reach terminal, makes equally plant factor reduce.The concentration of solution is preferably in 10-11(W/%).Even if like this, PVC is also just suspended in and is solvent swelling state in chlorobenzene.
The initiator of selecting includes but not limited to Diisopropyl azodicarboxylate, dilauroyl peroxide etc., the 0.1-0.2(W/% that its consumption is PVC).Existing compound method is first PVC to be suspended in chlorobenzene and then to add initiator, can make like this initiator skewness in PVC, finally occurs that reaction is uneven, and finished product dissolves in bad order.First the present invention is dissolved in initiator chlorobenzene and forms homogeneous solution, and then adds PVC to make suspension.
Suspension is to react in the enamel reactor stirring at band, and closed reactor is evacuated down to vacuum tightness 0.08Mpa, uses nitrogen vacuum breaker to normal pressure.Start to heat up, control 5 ℃/min of heat-up rate <, 3 ℃/min of < is better, preferably 2 ℃/min.During 35 ℃ of reactor temperatures, start logical chlorine, logical chlorine speed is no more than 120 liters/h with per kilogram PVC and is advisable, be no more than 100 liters/h better, be preferably 90 liters/h. when reactor temperature reaches 85-90 ℃, increasing chlorine flux is no more than 240 liters/h with per kilogram PVC and is advisable, be no more than 200 liters/h better, be preferably 150-170 liter/h. and with tail gas, substantially do not arrange chlorine and be advisable.When temperature of reaction reaches 90-95 ℃, stop heating up, because chlorination is thermopositive reaction (1458kj/kgPVC), when temperature reaches 108 ± 0.3 ℃ or 112 ± 0.3 ℃, open chuck water coolant and keep this temperature and logical chlorine dose.The finished product chlorinity is at 61-65(W/%). reaction end can be according to cumulative heat release, the logical chlorine dose of accumulative total or measure product during the solubleness (chlorinity is at 61-65(W/%) in acetone solubleness maximum) determine.Reach reaction end, stop logical chlorine.
Gained chlorated liquid also will be used 0.5mpa(gauge pressure) nitrogen blows acid, makes the free Cl in chlorated liquid
2, HCl reaches below 0.001 (W/%).Original process using normal pressure blows acid, and the time is long, nitrogen consumption is large, and the present invention adopts decompression to blow acid, in 0.1-0.001mpa(absolute pressure) acid of pressure blowing down, greatly reduce nitrogen consumption, shortened simultaneously and blown the acid time.
From chlorated liquid, Benzene Chloride solution is separated out, reclaimed to chlorinated polyvinyl chloride with hot water and carry out simultaneously, this is operate continuously.The hot water flow that enters Analytic Tower is chlorated liquid mass rate 50-100 times, 70-90 is doubly better, preferably 80 times, hot water temperature 98-100 ℃, steam flow should be chlorated liquid mass rate 0.7-2.5 times, 0.9-1.5 is doubly better, preferably 1 times, pressure 0.35-0.6mpa is more preferably 0.4-0.5mpa, preferably the steam of 0.45mpa enters steam injector as power, and chlorated liquid enters steam injector simultaneously, by the steam of rapid flow, is cut into tiny drop, enter among the hot water of Analytic Tower, separate out tiny chlorinated polyvinyl chloride particle and suspend in water.Benzene Chloride and water form 90.2 ℃ of azeotrope boiling points, and azeotropic forms (W/%) Benzene Chloride 71.6, and water 28.4. azeotrope steams and after cooling, forms each immiscible two-phase from tower top, the Benzene Chloride that static separation obtains reuse after drying.This will be very large processing power and consume a large amount of steam, cost rises and almost cannot bear.The present invention adopts decompression component distillation, in 0.1-0.001mpa(absolute pressure) reclaim Benzene Chloride under pressure, greatly reduce steam consumption, shortened Benzene Chloride recovery time simultaneously, economic benefit is very remarkable.
Example one:
Preparation paint chlorinated polyvinyl chloride.At 5m
3the enamel attached middle school that band stirs adds Benzene Chloride (Benzene Chloride content > 99.2 W/%, W/% moisture content≤5 * 10, polystream content≤0.65
-5massfraction) 3.96 tons, add 0.772 kilogram of Diisopropyl azodicarboxylate, start and stir until initiator is all dissolved among chlorobenzene.Slowly add the PVC(polymerization degree 900, oil absorbency 28) 396 kilograms, cover reaction kettle cover, polymeric kettle is evacuated down to vacuum tightness 0.08Mpa, with 0.1mpa nitrogen vacuum breaker to normal pressure.Start to heat up, control 2 ℃/min of heat-up rate.During 35 ℃ of reactor temperatures, start logical chlorine, logical chlorine speed is 36m
3/ h. is when reactor temperature reaches 90 ℃, and strengthening chlorine flux is 64m
3/ h. does not substantially arrange chlorine with tail gas and is advisable.When temperature of reaction reaches 95 ℃, stop heating up, when temperature continues to rise to 112 ℃, open chuck water coolant and keep this temperature and logical chlorine dose.Reaction end is that the solubleness of measure product in acetone is determined.Reach reaction end, stop logical chlorine.The finished product chlorinity is at 63.5(W/%).
Gained chlorated liquid 0.5mpa(gauge pressure) nitrogen is in 0.01mpa(absolute pressure) blow acid under pressure, final free Cl
2, HCl reaches 0.001 (W/%).
Chlorinated polyvinyl chloride in the chlorated liquid blowing after acid is separated out with hot water, reclaim Benzene Chloride simultaneously.The hot water flow that enters Analytic Tower is 352 tons/h, chlorated liquid mass rate 4m
3/ h, 98 ℃ of hot water temperatures, steam flow is that 4000 kilograms of (0.45mpa gauge pressure) Benzene Chloride and water form azeotrope, azeotrope steams and after cooling, forms each immiscible two-phase from tower top, the Benzene Chloride that static separation obtains reuse after drying.
The chlorinated polyvinyl chloride aqeous suspension obtaining, after centrifuge dehydration, fluidized drying, obtains finished product, meets HG2002-91 first grade standard.
Example two:
Prepare fiber chlorinated polyvinyl chloride.At 5m
3the enamel attached middle school that band stirs adds Benzene Chloride (Benzene Chloride content > 99.2 W/%, W/% moisture content≤5 * 10, polystream content≤0.65
-5massfraction) 3.916 tons, add 0.484 kilogram of Diisopropyl azodicarboxylate, start and stir until initiator is all dissolved among chlorobenzene.Slowly add the PVC(polymerization degree 1400, oil absorbency 32) 484 kilograms, cover reaction kettle cover, polymeric kettle is evacuated down to vacuum tightness 0.08Mpa, with 0.1mpa nitrogen vacuum breaker to normal pressure.Start to heat up, control 2 ℃/min of heat-up rate.During 35 ℃ of reactor temperatures, start logical chlorine, logical chlorine speed is 36m
3/ h. is when reactor temperature reaches 90 ℃, and strengthening chlorine flux is 64m
3/ h. does not substantially arrange chlorine with tail gas and is advisable.When temperature of reaction reaches 95 ℃, stop heating up, when temperature continues to rise to 108 ℃, open chuck water coolant and keep this temperature and logical chlorine dose.Reaction end is that the solubleness of measure product in acetone is determined.Reach reaction end, stop logical chlorine.The finished product chlorinity is at 64(W/%).
Gained chlorated liquid 0.5mpa(gauge pressure) nitrogen is in 0.01mpa(absolute pressure) blow acid under pressure, final free Cl
2, HCl reaches 0.001 (W/%).
Chlorinated polyvinyl chloride in the chlorated liquid blowing after acid is separated out with hot water, reclaim Benzene Chloride simultaneously.The hot water flow that enters Analytic Tower is 352 tons/h, chlorated liquid mass rate 4m
3/ h, 98 ℃ of hot water temperatures, steam flow is that 4000 kilograms of (0.45mpa gauge pressure) Benzene Chloride and water form azeotrope, azeotrope steams and after cooling, forms each immiscible two-phase from tower top, the Benzene Chloride that static separation obtains reuse after drying.
The chlorinated polyvinyl chloride aqeous suspension obtaining, after centrifuge dehydration, fluidized drying, obtains finished product, meets HG2002-91 first grade standard.
Claims (4)
1. the preparation method of chlorinated polyvinyl chloride for a paint, coating and fiber, it is characterized in that, described method comprises following technique: initiator is dissolved in solvent, PVC is dissolved in and in above-mentioned solution, forms PVC solution, reactor is vacuumized to deoxidation, pass into vaporization chlorine and carry out chlorination, then with nitrogen, blow acid and obtain conforming with the chlorated liquid that elutriation is used, with hot water, the resin after chlorination is separated out from solvent phase, again through dehydration, the dry supervinyi chloride resin that makes, by wet distillation, from water, isolate solvent Benzene Chloride, recycling; The selected polyvinyl chloride resin polymerization degree should, at 850-950, preferably 900, be 22-30g/100g, preferably 24-28g/100g to plasticizer absorption; The polyvinyl chloride resin polymerization degree should, at 1350-1450, preferably 1400, be 26-34g/100g, preferably 28-32g/100g to plasticizer absorption; Solvent includes but not limited to tetracol phenixin, ethylene dichloride, tetrachloroethane and Benzene Chloride etc., the most handy Benzene Chloride, Benzene Chloride content>=99.2 W/%, polystream content≤0.65 W/%, moisture content≤5 * 10
-5massfraction; PVC chlorination initiator used includes but not limited to Diisopropyl azodicarboxylate, dilauroyl peroxide, and Diisopropyl azodicarboxylate is more conventional, first initiator is dissolved in Benzene Chloride, and then adds polyvinyl chloride resin; Operation is carried out under anoxybiotic state, and closed reactor is evacuated down to vacuum tightness 0.08Mpa, uses nitrogen vacuum breaker to normal pressure; Temperature of reaction is respectively 108 ± 0.3 ℃ and 112 ± 0.3 ℃, controls 5 ℃/min of heat-up rate <, and 3 ℃/min of < is better, and preferably 2 ℃/min, reaches 90-95 ℃ and stop heating up; During 35 ℃ of reactor temperatures, start logical chlorine, logical chlorine speed is no more than 120 liters/h with per kilogram PVC and is advisable, be no more than 100 liters/h better, be preferably 90 liters/h. when reactor temperature reaches 85-90 ℃, increasing chlorine flux is no more than 240 liters/h with per kilogram PVC and is advisable, be no more than 200 liters/h better, optimum value is 150-170 liter/h; PVC chlorated liquid also will be used 0.5mpa(gauge pressure) nitrogen carries out vacuum and blows acid, at 0.1-0.001mpa, < 0.05mpa is better, preferably in 0.01mpa(absolute pressure) acid of pressure blowing down;
PVC Benzene Chloride solution also will carry out elutriation, and hot water (98-100 ℃) flow that enters Analytic Tower is chlorated liquid mass rate 50-100 times, and 70-90 is doubly better, preferably 80 times.
2. the preparation method of chlorinated polyvinyl chloride for a kind of paint according to claim 1, coating and fiber, is characterized in that the 0.1-0.2(W/% that the consumption of described initiator is PVC).
3. the preparation method of chlorinated polyvinyl chloride for a kind of paint according to claim 1, coating and fiber, it is characterized in that, the described Benzene Chloride stripping that also will reduce pressure reclaims, at 0.1-0.001mp, < 0.05mpa is better, preferably under 0.01mpa (absolute pressure) pressure, reclaims Benzene Chloride.
4. the preparation method of chlorinated polyvinyl chloride for a kind of paint according to claim 1, coating and fiber, it is characterized in that, described stripping steam flow used should be chlorated liquid mass rate 0.7-2.5 times, 0.9-1.5 is doubly better, preferably 1 times, pressure 0.35-0.6mpa, is more preferably 0.4-0.5mpa, preferably 0.45mpa.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10081687B2 (en) | 2015-07-29 | 2018-09-25 | Reliance Industries Limited | Process for chlorination of a polymer |
| CN116731224A (en) * | 2023-08-14 | 2023-09-12 | 山东亚大新材料有限公司 | Preparation method of chlorinated polyvinyl chloride |
-
2013
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Non-Patent Citations (2)
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| 周菊兴: "《合成树脂与塑料工艺》", 31 August 2000, article "氯化聚氯乙烯（过氯乙烯树脂）" * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10081687B2 (en) | 2015-07-29 | 2018-09-25 | Reliance Industries Limited | Process for chlorination of a polymer |
| CN116731224A (en) * | 2023-08-14 | 2023-09-12 | 山东亚大新材料有限公司 | Preparation method of chlorinated polyvinyl chloride |
| CN116731224B (en) * | 2023-08-14 | 2023-10-27 | 山东亚大新材料有限公司 | Preparation method of chlorinated polyvinyl chloride |
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Address after: 125001 No. 1 chemical Street, Lianshan District, Liaoning, Huludao Patentee after: LIAONING FANGDA ENGINEERING DESIGN CO., LTD. Address before: 125001 chemical Street, Lianshan District, Huludao, Liaoning Patentee before: Huludao Jinhua Chemical Engineering Design Co., Ltd. |