CN103554313B - The preparation method of a kind of paint, coating and fiber chlorinated polyvinyl chloride - Google Patents
The preparation method of a kind of paint, coating and fiber chlorinated polyvinyl chloride Download PDFInfo
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Abstract
The preparation method of a kind of paint, coating and fiber chlorinated polyvinyl chloride, relate to a kind of preparation method of chlorinated polyvinyl chloride, comprise following technique: initiator is dissolved in solvent, PVC is dissolved in above-mentioned solution and forms PVC solution, deoxidation is vacuumized to reactor, pass into vaporization chlorine and carry out chlorination, then blow with nitrogen the chlorated liquid that acid obtains conforming with elutriation, with hot water, the resin after chlorination is separated out from solvent phase, again through dehydration, dry obtained supervinyi chloride resin, from water, solvent Benzene Chloride is isolated, recycling by wet distillation; The present invention is with the PVC of high-quality for raw material, and selective chlorination benzene is solvent, carries out chlorination reaction, obtain the supervinyi chloride resin of the paint of high-quality, coating and fiber under initiator and certain temperature effect.Adopt and special blow acid and Benzene Chloride solvent recovery process technology and condition, the throughput of device increases considerably, and invests and steam consumption significantly reduces.Economic benefit is very 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 a kind of paint, coating and fiber chlorinated polyvinyl chloride.
Background technology
Paint, coating and fiber chlorinated polyvinyl chloride (also claiming supervinyi chloride resin) are chlorination modified obtained by polyvinyl chloride (PVC) resin, are 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.Polyvinyl chloride resin is after superchlorination, the irregularity of molecular chain arrangement increases, polarity increases, the solvability of resin is increased, just can be dissolved in the organic solvents such as ketone, ester class, chlorinated hydrocarbon, nitro class, toluene, dimethylbenzene under normal temperature, under heating state, dissolve in benzene, aniline, phthalic acid dibutyl ester, tetracol phenixin etc.; Chemical stability increases, thus improves the performance of the thermotolerance of material and the corrosion of acid-and base-resisting, salt, oxygenant etc.Improve the mechanical property of the heat-drawn wire of resin, cl content brings up to 61-65% by 56.7%, and vicat softening temperature is by 72-82 DEG C, and (bringing up to 90-125 DEG C), maximum operation (service) temperature can reach 110 DEG C, and life-time service temperature is 95 DEG C.
Supervinyi chloride resin can obtain 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 make filter cloth and special working suit, the medical shirt etc. of anti-chemical corrosion, also can obtain the special filter cloth of atomic industry by direct spraying.Chlorinated polyvinyl chloride fiber also can do ocean rope goods as fishing net, undersea cable crust etc.The non-blushing thinner in plastics, the tackiness agent of rubber item and engineering can be made, industrial putty etc.Because this chlorinated polyvinyl chloride has good electrical insulation capability, be widely used in electric utility as insulating material.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 the blended alloying of thermosetting resin fusion, improves the performance of material, makes it to become more superior engineering plastics.
The chlorinated polyvinyl chloride only having solubilisate chloridization process to produce just can be applicable to paint and coating applications, is also applicable to other purposes simultaneously.PVC is dissolved in certain solvent and forms PVC solution by so-called solubilisate chloridization process exactly, then under the existence of initiator, pass into vaporization chlorine and carry out chlorination, then blow with nitrogen the chlorated liquid that acid obtains conforming with elutriation, with water, the resin after chlorination is separated out from solvent phase, then through super-dry with obtained supervinyi chloride resin.Solvent recuperation is used again.Existing solubilisate chloridization process Problems existing 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 air distillation recycling design, steam consumption is high, the time is long.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of paint, coating and fiber chlorinated polyvinyl chloride, the method adopt PVC in the solution chlorination obtain the method for painting, coating and fiber chlorinated polyvinyl chloride also claim supervinyi chloride resin, the method makes the throughput of device increase considerably, 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 a kind of paint, coating and fiber chlorinated polyvinyl chloride, described method comprises following technique: initiator is dissolved in solvent, PVC is dissolved in above-mentioned solution and forms PVC solution, deoxidation is vacuumized to reactor, pass into vaporization chlorine and carry out chlorination, then blow with nitrogen the chlorated liquid that acid obtains conforming with elutriation, with hot water, the resin after chlorination is separated out from solvent phase, again through dehydration, dry obtained supervinyi chloride resin, from water, solvent Benzene Chloride is isolated, recycling by wet distillation; 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>=99.2W/%, polystream content≤0.65W/%, moisture content≤5 × 10
-5massfraction; PVC chlorination initiator used includes but not limited to Diisopropyl azodicarboxylate, dilauroyl peroxide, and Diisopropyl azodicarboxylate is more conventional, is first dissolved in Benzene Chloride by initiator, and then adds polyvinyl chloride resin; Operation is carried out under anoxybiotic state, and closed reactor is evacuated down to vacuum tightness 0.08Mpa, with nitrogen vacuum breaker to normal pressure; Temperature of reaction is respectively 108 ± 0.3 DEG C and 112 ± 0.3 DEG C, controls heat-up rate < 5 DEG C/min, < 3 DEG C/min better, preferably 2 DEG C/min.Reach 90-95 DEG C to stop heating up; Logical chlorine is started during reactor temperature 35 DEG C, 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 DEG C, 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 uses 0.5mpa(gauge pressure) nitrogen carries out vacuum and blows acid, better at 0.1-0.001mpa, < 0.05mpa, 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 DEG C) flow entering Analytic Tower is chlorated liquid mass rate 50-100 times, and 70-90 is doubly better, preferably 80 times.
The preparation method of described a kind of paint, coating and fiber chlorinated polyvinyl chloride, the consumption of described initiator is the 0.1-0.2(W/% of PVC).
The preparation method of described a kind of paint, coating and fiber chlorinated polyvinyl chloride, described Benzene Chloride also will carry out steam stripping at reduced pressure recovery, better at 0.1-0.001mp, < 0.05mpa, preferably in 0.01mpa(absolute pressure) reclaim Benzene Chloride under pressure.
The preparation method of described a kind of paint, coating and fiber chlorinated polyvinyl chloride, described stripping steam flow used should be chlorated liquid mass rate 0.7-2.5 doubly, 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 is with the PVC of high-quality for raw material, and selective chlorination benzene is solvent, carries out chlorination reaction, obtain the supervinyi chloride resin of the paint of high-quality, coating and fiber under initiator and certain temperature effect.Adopt and special blow acid and Benzene Chloride solvent recovery process technology and condition, the throughput of device increases considerably, and invests and steam consumption significantly reduces.Economic benefit is very considerable.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
The present invention be with the PVC of high-quality for raw material, select suitable solvent, adopt special Technology and condition, obtain 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 in environmental protection; Also can there is chlorination reaction while solvent made by ethylene dichloride and tetrachloroethane and generate many monochloroethane, make the recovery of solvent and reuse complicated.Only have Benzene Chloride (Benzene Chloride content > 99.2W/%, polystream content≤0.65W/% moisture content≤5 × 10
-5massfraction) the most applicable.One is that PVC solubleness in Benzene Chloride is comparatively large, and two is that the PVC chlorination reaction velocity be dissolved in Benzene Chloride is fast.Three is that 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 of-CHCl-unit composition
2-CHCl-) n, desirable chlorinated polyvinyl chloride should be every two-CH
2-CHCl-unit has a hydrogen atom to be replaced formation (-CHCl-CHCl-CH by chlorine
2-CHCl-CH
2-CHCl-) 1/3n structure, but be in fact far from being literally true, uneven chlorination makes the chlorinated polyvinyl chloride obtained all be greatly affected on 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 at 9-13.5(W/%).If solution is excessively rare, then reacts too fierce, easily cause chain rupture, make low-molecular weight polymer too much.Also can produce overchlorinated.Make plant factor reduce, the norm quota of consumption raises simultaneously; If strength of solution is too high, then react uneven, finished product dissolves in bad order, and the chlorination reaction time is long, does not slowly reach terminal, makes plant factor reduce equally.The concentration of solution is preferably at 10-11(W/%).Even if like this, PVC is also just suspended in chlorobenzene in solvent swelling state.
The initiator selected includes but not limited to Diisopropyl azodicarboxylate, dilauroyl peroxide etc., and its consumption is the 0.1-0.2(W/% of PVC).Existing compound method is first suspended in chlorobenzene by PVC and then adds initiator, can make initiator skewness in PVC like this, and final appearance reacts uneven, and finished product dissolves in bad order.First initiator is dissolved in chlorobenzene and forms homogeneous solution by the present invention, and then adds PVC and make suspension.
Suspension carries out reacting in the enamel reactor of band stirring, and closed reactor is evacuated down to vacuum tightness 0.08Mpa, with nitrogen vacuum breaker to normal pressure.Start to heat up, control heat-up rate < 5 DEG C/min, < 3 DEG C/min better, preferably 2 DEG C/min.Logical chlorine is started during reactor temperature 35 DEG C, 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 DEG C, 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 substantially do not arrange chlorine with tail gas and be advisable.When temperature of reaction reaches 90-95 DEG C, stop heating up, because chlorination is thermopositive reaction (1458kj/kgPVC), when temperature reaches 108 ± 0.3 DEG C or 112 ± 0.3 DEG C, 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 maximum according to solubleness when cumulative heat release, accumulative logical chlorine dose or measure product solubleness in acetone (chlorinity is at 61-65(W/%)) determine.Reach reaction end, stop logical chlorine.
Gained chlorated liquid also uses 0.5mpa(gauge pressure) nitrogen carries out blowing acid, makes the free Cl in chlorated liquid
2, HCl reaches 0.001 (W/%) below.Original technique adopts normal pressure to blow 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, shorten simultaneously and blow the acid time.
The precipitation of chlorinated polyvinyl chloride hot water, recovery Benzene Chloride solution are carried out from chlorated liquid, this is operate continuously simultaneously.The hot water flow entering Analytic Tower is chlorated liquid mass rate 50-100 times, 70-90 is doubly better, preferably 80 times, hot water temperature 98-100 DEG C, 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, is cut into tiny drop by the steam flowed fast, among the hot water entering Analytic Tower, separate out tiny chlorinated polyvinyl chloride particle and suspend in water.Benzene Chloride and water form azeotrope boiling point 90.2 DEG C, and azeotropic composition (W/%) Benzene Chloride 71.6, water 28.4. azeotrope steams from tower top and form each immiscible two-phase, the Benzene Chloride that static separation obtains reuse after drying after cooling.This will very large processing power consume a large amount of steam, and cost increase almost cannot be born.The present invention adopts decompression co-boiling distiling, in 0.1-0.001mpa(absolute pressure) reclaim Benzene Chloride under pressure, greatly reduce steam consumption, shorten Benzene Chloride recovery time simultaneously, economic benefit is very remarkable.
Example one:
Prepare paint chlorinated polyvinyl chloride.At 5m
3the enamel attached middle school that band stirs adds Benzene Chloride (Benzene Chloride content > 99.2W/%, polystream content≤0.65W/% moisture content≤5 × 10
-5massfraction) 3.96 tons, add Diisopropyl azodicarboxylate 0.772 kilogram, 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, vacuum tightness 0.08Mpa is evacuated down to polymeric kettle, with 0.1mpa nitrogen vacuum breaker to normal pressure.Start to heat up, control heat-up rate 2 DEG C/min.Start logical chlorine during reactor temperature 35 DEG C, logical chlorine speed is 36m
3/ h. is when reactor temperature reaches 90 DEG C, 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 DEG C, stop heating up, when temperature continues to rise to 112 DEG C, open chuck water coolant and keep this temperature and logical chlorine dose.Reaction end is that measure product solubleness is in acetone 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) carry out blowing acid under pressure, finally free Cl
2, HCl reaches 0.001 (W/%).
The chlorinated polyvinyl chloride hot water blown in the chlorated liquid after acid is separated out, reclaims Benzene Chloride simultaneously.The hot water flow entering Analytic Tower is 352 tons/h, chlorated liquid mass rate 4m
3/ h, hot water temperature 98 DEG C, steam flow is that 4000 kilograms of (0.45mpa gauge pressure) Benzene Chloride and water form azeotrope, and azeotrope steams from tower top and form each immiscible two-phase, the Benzene Chloride that static separation obtains reuse after drying after cooling.
The chlorinated polyvinyl chloride aqeous suspension obtained, 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 > 99.2W/%, polystream content≤0.65W/% moisture content≤5 × 10
-5massfraction) 3.916 tons, add Diisopropyl azodicarboxylate 0.484 kilogram, 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, vacuum tightness 0.08Mpa is evacuated down to polymeric kettle, with 0.1mpa nitrogen vacuum breaker to normal pressure.Start to heat up, control heat-up rate 2 DEG C/min.Start logical chlorine during reactor temperature 35 DEG C, logical chlorine speed is 36m
3/ h. is when reactor temperature reaches 90 DEG C, 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 DEG C, stop heating up, when temperature continues to rise to 108 DEG C, open chuck water coolant and keep this temperature and logical chlorine dose.Reaction end is that measure product solubleness is in acetone 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) carry out blowing acid under pressure, finally free Cl
2, HCl reaches 0.001 (W/%).
The chlorinated polyvinyl chloride hot water blown in the chlorated liquid after acid is separated out, reclaims Benzene Chloride simultaneously.The hot water flow entering Analytic Tower is 352 tons/h, chlorated liquid mass rate 4m
3/ h, hot water temperature 98 DEG C, steam flow is that 4000 kilograms of (0.45mpa gauge pressure) Benzene Chloride and water form azeotrope, and azeotrope steams from tower top and form each immiscible two-phase, the Benzene Chloride that static separation obtains reuse after drying after cooling.
The chlorinated polyvinyl chloride aqeous suspension obtained, after centrifuge dehydration, fluidized drying, obtains finished product, meets HG2002-91 first grade standard.
Claims (2)
1. a preparation method for paint and chloride coatings polyvinyl chloride, it is characterized in that, described method comprises following technique: be first dissolved in Benzene Chloride by initiator, and then adds polyvinyl chloride resin, and concentration is 9-13.5W/%; Deoxidation is vacuumized to reactor, pass into gasification chlorine and carry out chlorination, then blow with nitrogen the chlorated liquid that acid obtains conforming with elutriation, with hot water, the resin after chlorination is separated out from solvent phase, again through dehydration, dry obtained supervinyi chloride resin, from water, solvent is isolated, recycling by wet distillation; Selected should at 850-950 for the preparation of the paint polyvinyl chloride resin polymerization degree, be that 22-30g/100g, PVC chlorination initiator used comprises Diisopropyl azodicarboxylate, dilauroyl peroxide to plasticizer absorption; Operation is carried out under anoxybiotic state, and closed reactor is evacuated down to vacuum tightness 0.08MPa, with nitrogen vacuum breaker to normal pressure; Temperature of reaction is 112 ± 0.3 DEG C, controls heat-up rate < 5 DEG C/min, reaches 90-95 DEG C and stops heating up; Logical chlorine is started during reactor temperature 35 DEG C, logical chlorine speed is no more than 120 liters/h with per kilogram PVC, when reactor temperature reaches 85-90 DEG C, strengthen chlorine flux and be no more than 240 liters/h with per kilogram PVC, PVC chlorated liquid also carries out vacuum with nitrogen and blows acid, pressure is that 0.1-0.001mPa, PVC Benzene Chloride solution also will carry out elutriation, and the 98-100 DEG C of hot water flow entering Analytic Tower is chlorated liquid mass rate 50-100 times; The consumption of described initiator is the 0.1-0.2(W/% of PVC); Described Benzene Chloride also will carry out steam stripping at reduced pressure recovery, under 0.1-0.001mPa pressure, reclaim Benzene Chloride; Stripping steam flow used should be chlorated liquid mass rate 0.7-2.5 doubly, pressure is 0.35-0.6mPa.
2. a preparation method for fiber chlorinated polyvinyl chloride, is characterized in that, described method comprises following technique: be first dissolved in Benzene Chloride by initiator, and then adds polyvinyl chloride resin, and concentration is 9-13.5W/%; Deoxidation is vacuumized to reactor, pass into gasification chlorine and carry out chlorination, then blow with nitrogen the chlorated liquid that acid obtains conforming with elutriation, with hot water, the resin after chlorination is separated out from solvent phase, again through dehydration, dry obtained supervinyi chloride resin, from water, solvent is isolated, recycling by wet distillation; The polyvinyl chloride resin polymerization degree should at 1350-1450, is that 26-34g/100g, PVC chlorination initiator used comprises Diisopropyl azodicarboxylate, dilauroyl peroxide to plasticizer absorption; Operation is carried out under anoxybiotic state, and closed reactor is evacuated down to vacuum tightness 0.08MPa, with nitrogen vacuum breaker to normal pressure; Temperature of reaction is 108 ± 0.3 DEG C, controls heat-up rate < 5 DEG C/min, reaches 90-95 DEG C and stops heating up; Logical chlorine is started during reactor temperature 35 DEG C, logical chlorine speed is no more than 120 liters/h with per kilogram PVC, when reactor temperature reaches 85-90 DEG C, strengthen chlorine flux and be no more than 240 liters/h with per kilogram PVC, PVC chlorated liquid also carries out vacuum with nitrogen and blows acid, pressure is that 0.1-0.001mPa, PVC Benzene Chloride solution also will carry out elutriation, and the 98-100 DEG C of hot water flow entering Analytic Tower is chlorated liquid mass rate 50-100 times; The consumption of described initiator is the 0.1-0.2(W/% of PVC); Described Benzene Chloride also will carry out steam stripping at reduced pressure recovery, under 0.1-0.001mPa pressure, reclaim Benzene Chloride; Stripping steam flow used should be chlorated liquid mass rate 0.7-2.5 doubly, pressure is 0.35-0.6mPa.
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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. |