CN105622825B - Produce device and its production technology and the application of polyvinyl chloride interpolymer paste resin - Google Patents

Produce device and its production technology and the application of polyvinyl chloride interpolymer paste resin Download PDF

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Publication number
CN105622825B
CN105622825B CN201610208625.6A CN201610208625A CN105622825B CN 105622825 B CN105622825 B CN 105622825B CN 201610208625 A CN201610208625 A CN 201610208625A CN 105622825 B CN105622825 B CN 105622825B
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reaction kettle
polymerization reaction
tank
seed
blowpit
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CN105622825A (en
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陈淑艳
李学斌
汤守强
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Liaoning Fangda Engineering Design Co Ltd
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Liaoning Fangda Engineering Design Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F214/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
    • C08F214/02Monomers containing chlorine
    • C08F214/04Monomers containing two carbon atoms
    • C08F214/06Vinyl chloride
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0046Sequential or parallel reactions, e.g. for the synthesis of polypeptides or polynucleotides; Apparatus and devices for combinatorial chemistry or for making molecular arrays
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00Processes of polymerisation
    • C08F2/01Processes of polymerisation characterised by special features of the polymerisation apparatus used
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F218/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, of carbonic acid or of a haloformic acid
    • C08F218/02Esters of monocarboxylic acids
    • C08F218/04Vinyl esters
    • C08F218/08Vinyl acetate

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

The present invention relates to a kind of field of polyvinyl chloride interpolymer paste resin, particularly a kind of device and its production technology for producing polyvinyl chloride interpolymer paste resin.Head tank is connected with seed reactor and polymerization reaction kettle, seed reactor is connected by seed storage tank with polymerization reaction kettle, polymerization reaction kettle is connected with blowpit, blowpit is connected by removing tower with drying tower, stripper, blowpit, seed reactor and polymerization reaction kettle are connected with gas holder respectively, gas holder is connected with VCM recycling can, and seed reactor, polymerization reaction kettle, blowpit and drying tower are connected with waste water collection tank respectively, and waste water collection tank is connected with stripper.Production technology is controlled by DCS, is carried out as follows:Raw material is prepared, prepared by seed, polymerize afterwards, blowing reclaims defoaming, VC recovery is removed, is spray-dried, waste water continuously automatically processes;The final products obtained are used to producing laminate adhesive agent, preventing stone hitting automobile chassis coating, weave cotton cloth coating and required resin during substrate.

Description

Produce device and its production technology and the application of polyvinyl chloride interpolymer paste resin
Technical field
The present invention relates to a kind of field of polyvinyl chloride interpolymer paste resin, particularly a kind of production polyvinyl chloride copolymerization paste tree The device and its production technology of fat.
Background technology
Polyvinyl chloride(PVC)Paste resin as the term suggests be such a resin mainly so that paste forms are made to apply, Ren Menchang It is referred to as plasticized paste with such a paste, is a kind of unique liquid form of the igelite under rough.Paste resin often by Emulsion and microsuspending method are made, and its reaction equation is:
nCH2=CHCL——→(CH2-CHCL)n.
For PVC paste resin because granularity is fine, its quality has nonflowing character as talcum powder.PVC paste resin is same Stable suspension is agitated to form after plasticizer mixing, that is, PVC paste material is made, or makees PVC plasticized pastes, PVC colloidal sols, and People are exactly used for being processed into end article in this form.It is various according to different product needs, addition during paste producing Filler, diluent, heat stabilizer, foaming agent and light stabilizer etc..
Paste the development of Resin Industry, there is provided a kind of only heated new liquid material for being just changed into polrvinyl chloride product Material.This kind of liquid material configuration is convenient, and stable performance, easy to control, easy to use, product properties is excellent, chemical stability is good, tool There are certain mechanical strength, easy coloring etc., therefore be widely used in artificial leather, flooring laminate, medical, precision instrument production and meal Drink elastomeric glove, vinyl toy, soft trade mark, wallpaper, the leaching modeling industry of industry(Electronic handle medicine equipment, labor protection glove Deng), paint, foamed plastic, conveyer belt, the production of automobile decoration etc..
Compared with traditional suspending resin, PVC paste resin has advantages below:
(1)Process equipment is inexpensive;(2)Mould simple cheap;(3)It can be made into F-SP;(4)Foaming is easy;(5)Product Heated number is few, and can on a small quantity, multi items are produced.
Global paste PVC resin industry is developed with fast speed always, and particularly nearly ten years, production capacity is with yield in jump Formula increases, and increases in Asia particularly significant.2014, about 5,500,000 tons/year of whole world paste polyvinyl chloride resin aggregated capacity, Chinese production capacity About 710,000 tons, account for global aggregated capacity 13%.
Preparation method mainly has
1. emulsion method emulsion polymerization formula mainly has VCM, water, water soluble starter and emulsifying agent.Emulsion polymerization is to stirring It is required that very strict, initiation is carried out in aqueous phase, and usually used initiator is water soluble persulfates and sulfurous acid The oxidation-reduction system of salt, reaction speed are relevant with the addition speed and amount of reducing agent.Generally, emulsion polymerization obtains Serum particle diameter is less than 0.2 μm, in order to reach the purpose of increase serum particle diameter, develops emulsion seeded polymerization, makes serum particle diameter Increase to 1.0 μm or so.In emulsion polymerization, if the high polymer serum generated is present, control material proportioning and bar Part, in principle VCM only polymerize on the serum particle generated, without re-forming new particle;This high polymer generated Serum just looks like crystal seed, therefore referred to as emulsion seeding polymerization.Not only there is rational particle diameter, it is necessary to which there is appropriate particle diameter point Cloth, it can just obtain the PVC paste resin of function admirable.Emulsifying agent is critically important in emulsion polymerization, and quantity used determines initiator Population, and main function has been risen to the size of final serum particle.Especially when carrying out seed generation, speed is triggered using height Rate and low-concentration emulsifier are produced, and serum particle size distribution can be made to narrow.
Microsuspending method microsuspension polymerization is that a kind of newer method of PVC paste resin is made, and its flow is:It is first that VCM, oil is molten Property initiator, emulsifying agent and water stable emulsus is made of the method for mechanical homogenization(Particle diameter is at 1.0 μm or so), then gathered Close.The excellent flowability of the PVC paste resin produced in this way, emulsifier is few, the heat endurance and water-resistance of resin It is improved.The production technology need to pay special attention to following influence factor:From suitable compound emulsifying agent and particle Modifying agent system;The homogenizing of polymerization system component;Mixing speed;The ratio between water and VCM monomers are appropriate.Be in current world wide most For widely used method.
The content of the invention
It is an object of the invention to provide a kind of device for producing polyvinyl chloride interpolymer paste resin and its production technology and Using.
The device of the present invention adopts the following technical scheme that:
A kind of device for producing polyvinyl chloride interpolymer paste resin, including head tank, stripper, seed reactor, polymerization are anti- Answer kettle, gas holder, blowpit, drying tower, waste water collection tank, head tank is connected with seed reactor and polymerization reaction kettle, and seed is anti- Kettle is answered to be connected by seed storage tank with polymerization reaction kettle, polymerization reaction kettle is connected with blowpit, and blowpit is by removing tower with doing Dry tower connection, stripper, blowpit, seed reactor and polymerization reaction kettle are connected with gas holder respectively, gas holder and VCM Recycling can is connected, and seed reactor, polymerization reaction kettle, blowpit and drying tower are connected with waste water collection tank respectively, wastewater collection Groove is connected with stripper.
Optimal technical scheme is used by device:
Stripper is connected by equalization basin with measuring tank, and measuring tank is connected with fast mixed groove mixed slowly, and fast mixed groove mixed slowly is with neutralizing Groove is connected, and neutralization chamber, except groove is connected, is floated except groove is connected with sand filter and centrifuge respectively, in sand filter device and sewage disposal with floating The heart connects.
Head tank includes VAM tank, VCM tank, hot desalinized water tank, desalination water pot, emulsifying agent tank, urged Agent tank, initiator tank and buffer tank, head tank include VAM tank, VCM tank, hot desalinized water tank, de- Brine tank, emulsifying agent tank, catalyst tank, initiator tank and buffer tank, aforementioned base materials tank is respectively with seed reactor and polymerizeing Reactor connects.
The first automatic cleaning and spraying mechanism and first are provided with seed reactor and concentrates charge pipe, on polymerization reaction kettle It is provided with the second automatic cleaning and spraying mechanism and second and concentrates charge pipe, polymerization reaction kettle is closed jacket structured.
Dynamic defoaming machine is housed, dynamic defoaming machine is connected with static Defoaming machine, and static Defoaming machine connects with gas holder on blowpit Connect, the loop of static Defoaming machine is connected with blowpit.
Blowpit passes sequentially through smart wet crushing mill, thin wet crushing mill, serum delivery pump and serum mixing channel and removing Tower connects, and is provided with the Defoaming machine being connected with gas holder in removing tower, removing tower is connected by latex groove with drying tower, drying tower One section of bag hose, screen cloth, hopper, pulverizer, two sections of bag hoses are passed sequentially through to be connected with finished product bin.
Seed reactor is connected by seed storage tank with polymerization reaction kettle.
Anti-fouling agent tank and terminator tank are further equipped with device.
Technical scheme is used by production technology:
Controlled by DCS, carried out as follows:
, raw material prepare:
It is anti-as the poly- seed of charging addition for the first time that VCM of the VCM flask volume than 15% ~ 40% will be accounted for Answer in kettle and polymerization reaction kettle, VAM is added after polymerization reaction kettle has been fed in VCM and all added, ginseng With copolyreaction;Emulsifying agent, buffer, initiator are continuously added in seed reactor and polymerization reaction kettle, and catalyst is disposable Add in seed reactor and polymerization reaction kettle;
, seed prepare
Hot desalinized water is added in seed reactor, and emulsifying agent is added when reacting and starting, to form polyvinyl chloride particles, When seed reactor pressure drops to 4 to 6Kg/cm2When, VCM is added, when seed reactor pressure drop, cooling When valve is closed, polyvinyl chloride particles enter seed storage tank;
, rear polymerization:
Hot desalinized water is delivered in polymerization reaction kettle, is in proportion added aforementioned particles in polymerization reaction kettle by seed;Acetic acid Vinyl monomer all adds when seed reactor and polymerization reaction kettle add VCM for the first time;Reaction pressure will be Rate of polymerization declines after slowing down, and shows that polymerization terminates;
, blowing recovery defoaming:
When the pressure in polymerization reaction kettle is down to 0. 02~0.0 8Mpa, discharge of materials to blowpit is reclaimed and stored; Reclaimed using negative pressure, when pressure is down to 0. 02~0. 08Mpa in blowpit, start vavuum pump recovery, steam is passed through discharging Heated up inside groove, serum temperature reaches 40 DEG C~80 DEG C, and pressure reaches -400~-700mmH in blowpit2Terminate during O;
Serum is pumped into VC recovery defoamings from blowpit conveying;
Being carried out in blowpit from when pushing back receipts and negative pressure recovery, system can take the emulsifying agent and serum that foam includes out of, Defoaming treatment is carried out via dynamic defoaming machine and static Defoaming machine, the serum that is captured is pumped to drying again after returning to blowpit System is dried;
, VC recovery removing:
PVC serums in blowpit are sent in removing tower by spray nozzle, and after removing tower is heated with steam, serum is in removing tower It is interior to stop 3~6 hours, after removing, content of vinylchloride in serum by 2000~2200ppm be down to 200~300ppm with Under;
, spray drying:
Serum after being reclaimed by removing tower, which enters, to be dried in groove, and the serum dried in groove is entered back into drying tower, is done Resin after dry is collected into bag hose, is sent into warehouse for finished product;
, drying tower high pressure cleans automatically:
Drier is using the rinse water pressure control range used in automatic high pressure cleaning equipment:20~35Mpa;
, waste water continuously automatically processes:
The wastewater collection discharged from latex groove, polymerization reaction kettle, blowpit, drying tower is in waste water collection tank, waste water VC contents are in 3000-5000ppm in waste water in collecting tank;Waste water reclaims in waste water after stripping and remains VC, VC contents are down to 100 below ppm;Wastewater collection imports that air Self-pressurizing agri is floating to remove groove in waste water equalization basin after fast mixed slow mixed again, strikes off concentration Sludge, sludge pumping to centrifuge, dehydration is collected packed into mud cake after sell and floating deliver to sand filtration tank except rear waste water and carry out automatically Continuous processing, COD contents are down to below 200ppm, then deliver to wastewater treatment center processing.
Preferred scheme is used by production technology:
Emulsifying agent is divided into two kinds, and wherein emulsifier EM 1 is used for polymerization prepared by emulsion seed, and water dissolvable thing, in breast Agent groove, which is pre-dissolved, to be continuously added in seed reactor;Emulsifier EM 2 is used for the preparation of emulsion chlorine vinegar interpolymer paste resin, be it is a kind of with Water dissolvable thing, it is to be pre-dissolved to be continuously added in polymerization reaction kettle in emulsifying agent groove.
Catalyst is divided into two classes, catalyst AC1, is to be pre-dissolved with the material of water soluble in catalyst tank, is to pass through gravity Stream is disposable to be added in seed reactor;Catalyst AC2, it is with being pre-dissolved in the pre- fluid bowl of the material of water soluble, is to pass through gravity stream It is disposable to add in reactor.
Buffer is divided into two kinds, is added to seed reactor and polymerisation simultaneously after the mixing of both phosphoric acid and caustic soda Kettle, to ensure pH 7 ~ 8.
Initiator is divided into two kinds, and initiator CAT1 is prepared for seed, and it is a kind of and water dissolvable peroxidating Thing, it is to be pre-dissolved to be continuously added in seed reactor in initiator tank;Initiator CAT2 is to be used for emulsion chlorine vinegar interpolymer paste resin system Standby, it is a kind of and water dissolvable peroxide, is to be pre-dissolved to be continuously added in polymerization reaction kettle in initiator tank.
Seed reactor and polymerization reaction kettle are also connected with anti-fouling agent tank respectively, and anti-fouling agent passes through 1.2 ~ 2.0Mpa Steam jet ejector sprays into seed reactor and polymerization reaction kettle, and fog is produced in kettle, makes the institute of biologically active prod covering reactor There is inwall.
In the case where polymerizeing out-of-control condition, terminator terminating reaction process is injected;Seed reactor and polymerization reaction kettle are matched somebody with somebody respectively Two terminator tanks are had, two terminator tanks are 1.6 ~ 2.5MPa nitrogen seal pressures.
Before vinyl chloride condensation, recovery vinyl chloride is handled with stabilizer and liquid caustic soda.
Production laminate adhesive agent, preventing stone hitting automobile chassis coating, weave cotton cloth coating and substrate when required resin.
Brief description of the drawings
Fig. 1 is the process flow diagram of the present invention.
Embodiment
Below in conjunction with the accompanying drawings and the present invention is described in detail in embodiment:
A kind of device for producing polyvinyl chloride interpolymer paste resin, referring to accompanying drawing 1, in figure:Sand filter 1, float except groove 2, neutralize Groove 3, fast mixed groove 4 mixed slowly, measuring tank 5, equalization basin 6, stripper 7, the first centrifuge 8, the first vavuum pump 9, waste water collection tank 10, Buffer tank 11, initiator tank 12, catalyst tank 13, emulsifying agent tank 14, desalination water pot 15, hot desalinized water tank 16, vinyl chloride list Body storage tank 17, VAM tank 18, VCM recycling can 19, the second centrifuge 24, the 3rd centrifuge the 25, the 4th from Scheming 26, the 5th centrifuge 27, the 6th centrifuge 28, the first seed storage tank 29, second seed storage tank 30, seed reactor 31, First concentrates the automatic cleaning of charge pipe 32, first and the automatic cleaning of spraying mechanism 33, second and spraying mechanism 34, second to concentrate and add Expects pipe 35, polymerization reaction kettle 36, the second vavuum pump 37, rectifier unit 38, gas holder 39, static defoaming mechanism 40, dynamic defoaming machine Structure 41, blowpit 42, smart wet crushing mill 43, thin wet crushing mill 44, serum delivery pump 45, the 3rd vavuum pump 46, first steam Vapour knockout drum 47A, the first serum mixing channel 48A, the first Defoaming machine 49A, the first removing tower 50A, the second steam knockout drum 48A, Second serum mixing channel 48B, the second Defoaming machine 49B, the second removing tower 50B, latex groove 51, serum constant displacement pump 52, drying tower 53rd, pulverizer 54, hopper 55,56, one sections of filter screen 57, two sections of bag hose bag hose 58, finished product bin 59, automatic packaging system 60。
In the present embodiment, head tank is connected with seed reactor 31 and polymerization reaction kettle 36, and head tank includes vinyl acetate Monomer tank 18, VCM tank 17, hot desalinized water tank 16, desalination water pot 15, emulsifying agent tank 14, catalyst tank 13, initiator Tank 12 and buffer tank 11, head tank are connected with seed reactor 31 and polymerization reaction kettle 36 respectively.Seed reactor 31 passes through First seed storage tank 39 and second seed storage tank 30 are connected with polymerization reaction kettle 36, and polymerization reaction kettle 36 is connected with blowpit 42, Blowpit 42 passes sequentially through thick wet crushing mill 43, thin wet crushing mill 44, serum delivery pump 45, the first serum mixing channel 48A It is connected with the first removing tower 50A;First removing tower 50A is connected with the second serum mixing channel 48B, and the first serum closes mixing channel 48A On be connected with the first steam knockout drum 47A, the second serum, which closes, is connected with the second steam knockout drum 47B on mixing channel 48B, first is de- Except being equipped with tower 50A on the first Defoaming machine 49A, the second removing tower 50B equipped with the second Defoaming machine 49B, the first Defoaming machine 49A and Second Defoaming machine 49B is connected with gas holder 39 respectively;Blowpit 42 is connected by the second removing tower 50B with drying tower 53.
Stripper 7, blowpit 42, seed reactor 31 and polymerization reaction kettle 36 are connected with gas holder 39 respectively, gas holder 39 with VCM recycling can 19 connects, seed reactor 31, polymerization reaction kettle 36, blowpit 42 and drying tower 53 respectively with waste water Collecting tank 10 is connected, and waste water collection tank 10 is connected with stripper 7.
Stripper 7 is connected by equalization basin 6 with measuring tank 5, and measuring tank 5 is connected with fast mixed groove 4 mixed slowly, fast mixed groove 4 mixed slowly It is connected with neutralization chamber 3, neutralization chamber 3, except groove 2 is connected, is floated except groove 2 is connected with the centrifuge 8 of sand filter 1 and first respectively, sand filtration with floating Device 1 is connected with treatment center of sewage.
The first automatic cleaning is provided with seed reactor 31 and spraying mechanism 33 and first concentrates charge pipe 32, polymerization is instead Answer and the second automatic cleaning and the concentration charge pipe 35 of spraying mechanism 34 and second are provided with kettle 36, polymerization reaction kettle 36 is closed folder Nested structure.
Dynamic defoaming machine 41 is housed, dynamic defoaming machine 41 is connected with static Defoaming machine 40, static Defoaming machine on blowpit 42 40 are connected with gas holder 39, and the loop of static Defoaming machine 40 is connected with blowpit 42.
Second removing tower 50B is connected by latex groove 51 with drying tower 53, and drying tower 53 passes sequentially through one section of bag hose 57th, 54, two sections of screen cloth 56, hopper 55, pulverizer bag hoses 58 are connected with finished product bin 59;Finished product bin 60 and automatic packaging system The connection of system 60.
Anti-fouling agent tank and terminator tank are further equipped with device;Anti-fouling agent tank and terminator tank react with seed respectively Kettle connects with polymerization reaction kettle.
The production technology of embodiment 1,2, whole production process are controlled by DCS, are carried out as follows:
Present apparatus consersion unit is stainless steel cauldron:The volume of seed reactor 31 is 30~55 cubic metres, for planting The preparation of son;The volume of polymerization reaction kettle is 65~90 cubic metres;The present embodiment selects 80 cubic metres of polymerization reaction kettle 36, Seed reactor is using 35 cubic metres.
The present embodiment stores emulsion seed by two seed reactors, and during actual production, a collection of polymerization only uses very little A kind of seed of percentage, every batch of dosage is at 3~5 tons or so;Batch of seeds can be used for three batches of polymerisations;Number prepared by seed Quantity of the amount depending on seed in daily polymerisation number and seed storage tank.
Embodiment 1:
, raw material prepare:
20% in VCM cumulative volume will be filled in VCM storage tank 17(About 30 ~ 35 cubic metres), make Added to feed for the first time in seed reactor 31 and polymerization reaction kettle 36, afterwards for being continuously added to materials during polymerisation, The vinyl chloride reclaimed in vinyl chloride recycling can 19 feeds as another part of seed reactor 31 and polymerization reaction kettle 36 and added.
About 1200 ~ 1500Kg VAM adds addition polymerization reaction kettle 36 for the first time in VCM and entered All added after having expected, participate in copolyreaction;Emulsifying agent about 650 ~ 800Kg, buffer about 1200 ~ 1500Kg, initiator About 8 ~ 12Kg is continuously added in seed reactor 31 and polymerization reaction kettle 36;Foregoing emulsifying agent, buffer and initiator difference It is continuously added to by both volume ratios by seed reactor 31 and polymerization reaction kettle 36;Catalyst about 15 ~ 22Kg disposably adds Enter in seed reactor 31 and polymerization reaction kettle 36;Catalyst is also added by the volume ratio of seed reactor 31 and polymerization reaction kettle 36 Enter.
Emulsifying agent is divided into two kinds, and wherein emulsifier EM 1 is used for polymerization prepared by emulsion seed, and water dissolvable thing, in breast Agent groove, which is pre-dissolved, to be continuously added in seed reactor 31;Emulsifier EM 2 is used for the preparation of emulsion chlorine vinegar interpolymer paste resin, is a kind of It is to be pre-dissolved to be continuously added in polymerization reaction kettle 36 in emulsifying agent groove with water dissolvable thing.
Catalyst is divided into two classes, catalyst AC1, is and water-soluble substance, is pre-dissolved in catalyst tank, is by gravity stream one Secondary property is added in seed reactor 31;Catalyst AC2, it is pre-dissolved with the mode similar to emulsifying agent in pre- fluid bowl, is to pass through gravity Stream is disposable to be added in polymerization reaction kettle 36.
Two kinds of buffers:Phosphoric acid and caustic soda, both buffers respectively account for total 50% or so volume ratio, quilt after both mix It is added in seed reactor 31 and polymerization reaction kettle 36, phosphoric acid and caustic soda press boths' of seed reactor and polymerization reaction kettle Volume ratio is added in seed reactor 31 and poly- full response kettle 36, to ensure pH values between 7 ~ 8.
Initiator:Initiator is divided into two kinds, and initiator CAT1 is prepared for seed, and it is a kind of and water dissolvable Peroxide, be to be pre-dissolved to be continuously added in seed reactor in initiator tank.
Initiator CAT2 is prepared for emulsion chlorine vinegar interpolymer paste resin, and it is a kind of and water dissolvable peroxidating Thing, it is to be pre-dissolved to be continuously added in polymerization reaction kettle in initiator tank.
Seed reactor 31 and polymerization reaction kettle 36 are also connected with anti-fouling agent tank respectively, anti-fouling agent by 1.2 ~ 2.0Mpa steam jet ejectors are sprayed into seed reactor 31 and polymerization reaction kettle 36, and fog is produced in kettle, covers biologically active prod All inwalls of lid reactor.
In the case where polymerizeing out-of-control condition, terminator terminating reaction process is injected.Seed reactor and polymerization reaction kettle are matched somebody with somebody respectively Two terminator tanks are had, two terminator tanks are 1.6 ~ 2.5MPa nitrogen seal pressures.
Before vinyl chloride condensation, recovery vinyl chloride is handled with stabilizer and liquid caustic soda.
, seed prepare
It is defeated with the pump of the second centrifugal pump 25 out of hot desalinized water tank 16 that hot desalinized water accounts for the 0.8 ~ 1.4% of VCM volume Deliver in seed reactor 31, emulsifying agent is added when reacting and starting, and to form polyvinyl chloride particles, other additives pass through In centrifugal pump seed injection reactor 31.Before adding vinyl chloride, the air in emptying reactor is anti-by seed with initial vacuum pump Kettle 31 is answered to vacuumize;When seed reactor pressure declines about 5Kg/cm2When, VCM is added, when seed reactor 31 is pressed When power drop, cooling valve are closed, polyvinyl chloride particles respectively enter the first seed storage tank 29 and second seed storage tank 30.
When loading VCM rises, polymerization cycle starts to start;When seed reactor pressure declines, cooling valve is closed When, after polymerization terminates, reclaim naturally, when seed reactor pressure is down to 0, enters by filter and respectively enter the first seed storage tank 29 and second seed storage tank 30 stored;And it is standby to analyze particle size.
Afterwards, quick, the safe closed pressure pressure cleaning automatically of the inside of seed reactor 31 progress, high-pressure water pressure 25~ 35Mpa, used again in closed after the completion of cleaning and press automatic spray to rinse, seed reactor 31 carries out fountain flushing, pressure model Enclose:2.5~4.0 MPa.Feeding tube cleaning systems are carried out afterwards, carry out the closed automatic spraying of seed reactor anti-adhesion agent afterwards, Wait next batch reaction operation;Wherein waste water is unified collects in waste water collection tank 10.
The temperature operating ranges of seed reactor 31:45~55 DEG C;The purging system of seed reactor 31, spray irrigation and anti-stick Agent spraying is controlled using DCS, and the cleaning of seed reactor is entered to be carried out using desalted water.
, rear polymerization:
Hot desalinized water accounts for the 0.8 ~ 1.4% of VCM volume out of hot desalinized water tank 16, is sent by the 3rd centrifugal pump 25 Into polymerization reaction kettle 36, add after hot desalinized water after 5, the emulsion seed as made from 8% ~ 18% by aforementioned particles adds polymerization In reactor 36, other additives(Emulsifying agent, catalyst, initiator, buffer etc.)Add simultaneously in polymerization reaction kettle 36, its Middle initiator(CAT2, depending on the trade mark)Use, be by reaction release heat control;Added by the temperature of reactor to control Enter the flow velocity of initiator.
For polymerization, only the VCM of volume ratio 15% ~ 40% is being initially added, and remaining VCM is Added in polymerization process, the flow for being continuously added to vinyl chloride is determined according to reaction rate;Reactor operating condition by In the different and different of production product grade.
VAM all adds when seed reactor 31 and polymerization reaction kettle 36 add VCM for the first time Enter;Reaction pressure will decline after rate of polymerization slows down, and show that polymerization terminates.When the pressure of polymerization reaction kettle 36 is down to 0.2~ During 0.6Mpa, discharge of materials to blowpit is reclaimed and stored.
Afterwards, the automatic cleaning of quick, safety closed pressure pressure, high-pressure water pressure 25 are carried out to the inside of polymerization reaction kettle 36 ~35Mpa, used again in closed after the completion of cleaning and press automatic spray to rinse, seed reactor 36 carries out fountain flushing, pressure Scope:2.5~4.0 MPa.Feeding tube cleaning systems are carried out in next step, and it is closed certainly to carry out the anti-adhesion agent of polymerization reaction kettle 36 afterwards Dynamic spraying, wait next batch reaction operation;Wherein waste water is unified collects in waste water collection tank 10.
The chuck form of polymerization reaction kettle 36:Total closed type;36 special whipped form of polymerization reaction kettle:Two layers of three leaves stirrings Structure.
Polymerization reaction kettle 36 cleaned, be sprayed and anti-adhesion agent spraying is controlled using DCS, and desalted water is used to carrying out clear Wash.
, blowing recovery defoaming:
When the pressure in polymerization reaction kettle 36 is down to 0. 02~0.0 8Mpa, discharge of materials to blowpit 42 is reclaimed Storage;Reclaimed using from pressure and negative pressure, when pressure is down to 0. 02~0. 08Mpa in blowpit 42, start vacuum Blowback is received, and steam is passed through inside blowpit 42 and heated up, and serum temperature reaches 40 DEG C~80 DEG C, and pressure reaches in blowpit 42 Terminate during to -0.052 ~ 0.092Mpa;The state of 42 inclined placement of blowpit, the angle between horizontal plane is about 5~ 10 degree.
Serum is sent in the first serum mixing channel 48A from blowpit 42 by serum delivery pump 45, the first serum mixing channel 48A is connected with the first VC removing towers 50A;First VC removing towers 50A is connected with the second serum mixing channel 48B, the mixing of the second serum Groove 48B is connected with the 2nd VC removing towers 50B.
Carried out in blowpit 42 from when pushing back receipts and negative pressure recovery, system can take the emulsifying agent and breast that foam includes out of Slurry, defoaming treatment is carried out via dynamic defoaming machine 41 and static Defoaming machine 40(Dynamic defoaming machine 41, specification EM-431, Kunshan is forever Win Products;Static Defoaming machine 40, model:EC-431), this defoaming mode can not use defoamer and can complete, Improve final product quality, be advantageous to downstream production, the serum that is captured return to after blowpit 42 again by thick wet crushing mill 43, Thin wet crushing mill 44 and serum delivery pump 45 are delivered to after VC removing towers are removed and are dried into drying tower 53.
The VC contents of serum tentatively can be down to below 2000ppm by the step by 16000~20000ppm, reclaimed big The VC of amount, reduce VC unit consumption.
, VC recovery removing:
PVC serums in blowpit 42 are pumped in the first VC removing towers 50A by spray nozzle by serum conveying, make PVC Serum can be suitably distributed in tower wall, and temperature and vacuum in control tower.PVC breasts through first order removing tower 50A removings Slurry is from bottom of towe pipeline via being pumped into the 2nd VC removing towers 50B.Before second level removing tower is added, PVC serums pass through heating If reserve steam is heated to control temperature.After two-stage removes, the content of vinylchloride in serum is down to by about 2000ppm Below 300ppm.
After first VC removing towers are heated with steam, vapor (steam) temperature is controlled at 50~80 DEG C.Serum is in two level removing tower Residence time is 3~6 hours, after two level removes, content of vinylchloride in serum is down to 200 by 2000~2200ppm~ Below 300ppm.VC monomers have further been reclaimed, have reduced VC unit consumption, can have been made in follow-up drying process exhaust outlet emission VC contents are less than below 10ppm, and package unit will be more environmentally-friendly.Vacuum degree control scope in removing tower:- 400~-700 mmHg (About -0.004~-0.007Mpa).
, spray drying:
Serum after being reclaimed by the 2nd VC removing towers 50B enters in serum groove 51, and the serum in serum groove 51 enters again Enter in drying tower 53, dried resin sequentially enters pulverizer 54 into one section of bag hose 57, filter screen 56 and hopper 55 and carried out Crushed work, malleation discharge pressure control range is conveyed with malleation:3000~5000mmHg(About 0.03~-0.05Mpa)To into Product feed bin 57, malleation fed distance can make the integral arrangement of dry, packaging and finished room more flexible, warp up to 200m or so Warehouse for finished product is sent into after automatic packaging system 60, automatic packaging system 60 uses open type or port type automatic packaging system.
, drying tower high pressure cleans automatically:
Drier is using the rinse water pressure control range used in automatic high pressure cleaning equipment:20~35Mpa;Spray drying Device operation can be attached in tower wall through slurry after a period of time, can be dropped in producing and be polluted paste resin finished product and shadow Quality is rung, so a period of time effectively can clean up tower wall Xu Let via automatic high pressure cleaning equipment surely(Pass through desalination Water cleans);Rinse water pressure control range used in the automatic high pressure cleaning equipment of the automatic cleaning step of drying tower high pressure:20~ 35Mpa;The automatic cleaning step of drying tower high pressure, labor intensity can be greatly lowered, improve final product quality and yield rate.
, waste water continuously automatically processes:The continuous automated processing system of waste water is controlled by DCS, reduces labor intensity.
The wastewater collection discharged from latex groove 51, polymerization reaction kettle 36, blowpit 42, drying tower is in waste water collection tank 10 In, VC contents are in 3000~5000ppm in the waste water in waste water collection tank 10;Waste water reclaims in waste water after stripping and remains VC, VC contents are down to 100 below ppm;Waste water(COD contents 2000-3000ppm, SS content 3000-5000ppm)It is collected in waste water Equalization basin 6 is again through fast mixed groove 4 mixed slowly(Mixed 80~100 revs/min of revolution soon)Enter afterwards in neutralization chamber 3, enter again from neutralization chamber 3 It is floating except in groove 2, automatic scraping is except the sludge of concentration, sludge pumping to the automatic dehydration of the first centrifuge 8, dehydration to enter air Self-pressurizing agri Sold after collecting into mud cake packaging, floating to deliver to sand filtration tank 1 except rear waste water and automatically continuously handled, COD contents are down to 200ppm Hereinafter, then wastewater treatment center processing is delivered to.
The final products that the technique of the present invention is obtained, are applied to:Produce laminate adhesive agent, preventing stone hitting automobile chassis applies Layer, weave cotton cloth coating and required resin during substrate.
The bottom injection steam of waste water collection tank 10, injects from waste water pot bottom;The operating condition of steam:Temperature 80~98 DEG C, pressure -400~-700mmH2O(About -0.004~-0.007Mpa).
Embodiment 2:
The production technology of the present embodiment, whole production process are controlled by DCS, are carried out as follows:
Present apparatus consersion unit is stainless steel cauldron:The volume of seed reactor 31 is 30~55 cubic metres, for planting The preparation of son;The volume of polymerization reaction kettle is 65~90 cubic metres;The present embodiment selects 80 cubic metres of polymerization reaction kettle 36, Seed reactor is using 35 cubic metres.
The present embodiment stores emulsion seed by two seed reactors, and during actual production, a collection of polymerization only uses very little A kind of seed of percentage, every batch of dosage is at 3~5 tons or so;Batch of seeds can be used for three batches of polymerisations;Number prepared by seed Quantity of the amount depending on seed in daily polymerisation number and seed storage tank.
, raw material prepare:
20% in VCM cumulative volume will be filled in VCM storage tank 17(About 30 cubic metres), as Once charging is added in seed reactor 31 and polymerization reaction kettle 36, afterwards for being continuously added to materials, chloroethene during polymerisation The vinyl chloride reclaimed in alkene recycling can 19 feeds as another part of seed reactor 31 and polymerization reaction kettle 36 and added.
VAM VCM add for the first time after polymerization reaction kettle 36 has been fed all add it is poly- complete In reactor 36, copolyreaction is participated in;Emulsifying agent 650Kg, buffer 1200Kg, initiator 8Kg are continuously added to seed reactor 31 and polymerization reaction kettle 36 in;Foregoing emulsifying agent, buffer and initiator are respectively by pressing seed reactor 31 and polymerization reaction kettle 36 both volume ratios are continuously added to;Catalyst about 15Kg is disposably added in seed reactor 31 and polymerization reaction kettle 36; The volume ratio that catalyst also presses seed reactor 31 and polymerization reaction kettle 36 adds.
Emulsifying agent is divided into two kinds, and wherein emulsifier EM 1 is used for polymerization prepared by emulsion seed, and water dissolvable thing, in breast Agent groove, which is pre-dissolved, to be continuously added in seed reactor 31;Emulsifier EM 2 is used for the preparation of emulsion chlorine vinegar interpolymer paste resin, is a kind of It is to be pre-dissolved to be continuously added in polymerization reaction kettle 36 in emulsifying agent groove with water dissolvable thing.
Catalyst is divided into two classes, catalyst AC1, is and water-soluble substance, is pre-dissolved in catalyst tank, is by gravity stream one Secondary property is added in seed reactor 31;Catalyst AC2, it is pre-dissolved with the mode similar to emulsifying agent in pre- fluid bowl, is to pass through gravity Stream is disposable to be added in polymerization reaction kettle 36.
Two kinds of buffers:Phosphoric acid and caustic soda, both buffers respectively account for total 50% or so volume ratio, quilt after both mix It is added in seed reactor 31 and polymerization reaction kettle 36, phosphoric acid and caustic soda press boths' of seed reactor and polymerization reaction kettle Volume ratio is added in seed reactor 31 and poly- full response kettle 36, to ensure pH values 7 or so.
Initiator:Initiator is divided into two kinds, and initiator CAT1 is prepared for seed, and it is a kind of and water dissolvable Peroxide, be to be pre-dissolved to be continuously added in seed reactor in initiator tank.
Initiator CAT2 is prepared for emulsion chlorine vinegar interpolymer paste resin, and it is a kind of and water dissolvable peroxidating Thing, it is to be pre-dissolved to be continuously added in polymerization reaction kettle in initiator tank.
Seed reactor 31 and polymerization reaction kettle 36 are also connected with anti-fouling agent tank respectively, anti-fouling agent by 1.2 ~ 2.0Mpa steam jet ejectors are sprayed into seed reactor 31 and polymerization reaction kettle 36, and fog is produced in kettle, covers biologically active prod All inwalls of lid reactor.
In the case where polymerizeing out-of-control condition, terminator terminating reaction process is injected.Seed reactor and polymerization reaction kettle are matched somebody with somebody respectively Two terminator tanks are had, two terminator tanks are 1.6 ~ 2.5MPa nitrogen seal pressures.
Before vinyl chloride condensation, recovery vinyl chloride is handled with stabilizer and liquid caustic soda.
, seed prepare
Hot desalinized water accounts for the 0.8% of VCM volume out of hot desalinized water tank 16, is delivered to the pump of the second centrifugal pump 25 In seed reactor 31, emulsifying agent is added when reacting and starting, and to form polyvinyl chloride particles, other additives pass through centrifugation In pump seed injection reactor 31.Before adding vinyl chloride, the air in emptying reactor, with initial vacuum pump by seed reactor 31 vacuumize;When seed reactor pressure declines about 5Kg/cm2When, add VCM, when the pressure drop of seed reactor 31, When cooling down valve closing, polyvinyl chloride particles respectively enter the first seed storage tank 29 and second seed storage tank 30.
When loading VCM rises, polymerization cycle starts to start;When seed reactor pressure declines, cooling valve is closed When, after polymerization terminates, reclaim naturally, when seed reactor pressure is down to 0, enters by filter and respectively enter the first seed storage tank 29 and second seed storage tank 30 stored;And it is standby to analyze particle size.
Afterwards, the automatic cleaning of quick, safety closed pressure pressure, high pressure are carried out by desalted water inside seed reactor 31 25~35Mpa of water pressure, used again in closed after the completion of cleaning and press automatic spray to rinse, seed reactor 31 carries out fountain punching Wash, pressure limit:2.5~4.0 MPa.Feeding tube cleaning systems are carried out afterwards, and it is closed to carry out seed reactor anti-adhesion agent afterwards Automatic spraying, wait next batch reaction operation;Wherein waste water is unified collects in waste water collection tank 10.
The temperature operating ranges of seed reactor 31:45~55 DEG C;The purging system of seed reactor 31, spray irrigation and anti-stick Agent spraying is controlled using DCS, and the cleaning of seed reactor is entered to be carried out using desalted water.
, rear polymerization:
Hot desalinized water accounts for the 0.8 ~ 1.4% of VCM volume out of hot desalinized water tank 16, is sent by the 3rd centrifugal pump 25 Into polymerization reaction kettle 36, add after hot desalinized water after 5, it is anti-that the emulsion seed as made from 8% ~ 18% by aforementioned particles adds polymerization Answer in kettle 36, other additives(Emulsifying agent, catalyst, initiator, buffer etc.)Add simultaneously in polymerization reaction kettle 36, wherein Initiator(CAT2, depending on the trade mark)Use, be by reaction release heat control;Added by the temperature of reactor to control The flow velocity of initiator.
For polymerization, only the VCM of volume ratio 15% ~ 40% is being initially added, and remaining VCM is Added in polymerization process, the flow for being continuously added to vinyl chloride is determined according to reaction rate;Reactor operating condition by In the different and different of production product grade.
VAM all adds when seed reactor 31 and polymerization reaction kettle 36 add VCM for the first time Enter in polymerization reaction kettle 36;Reaction pressure will decline after rate of polymerization slows down, and show that polymerization terminates.When polymerization reaction kettle 36 When pressure is down to 0.2~0.6Mpa, discharge of materials to blowpit 42 is reclaimed into storage.
Afterwards, it is high to carrying out the automatic cleaning of quick, safety closed pressure pressure by desalted water inside polymerization reaction kettle 36 25~35Mpa of water pressure is pressed, is used again in closed after the completion of cleaning and presses automatic spray to rinse, seed reactor 36 carries out fountain Rinse, pressure limit:2.5~4.0 MPa.Feeding tube cleaning systems are carried out in next step, and it is anti-stick to carry out polymerization reaction kettle 36 afterwards The closed automatic spraying of agent, waits next batch reaction operation;Wherein waste water is unified collects in waste water collection tank 10.
The chuck form of polymerization reaction kettle 36:Total closed type;36 special whipped form of polymerization reaction kettle:Two layers of three leaves stirrings Structure.
Polymerization reaction kettle 36 cleaned, be sprayed and anti-adhesion agent spraying is controlled using DCS, and desalted water is used to carrying out clear Wash.
, blowing recovery defoaming:
When the pressure in polymerization reaction kettle 36 is down to 0. 02~0.0 8Mpa, discharge of materials to blowpit 42 is reclaimed Storage;Reclaimed using from pressure and negative pressure, when pressure is down to 0. 02~0. 08Mpa in blowpit 42, start vacuum Blowback is received, and steam is passed through inside blowpit 42 and heated up, and serum temperature reaches 40 DEG C~80 DEG C, and pressure reaches in blowpit 42 Terminate during to -0.052 ~ 0.092Mpa;The state of 42 inclined placement of blowpit, the angle between horizontal plane is about 5~ 10 degree.
Serum is sent in the first serum mixing channel 48A from blowpit 42 by serum delivery pump 45, the first serum mixing channel 48A is connected with the first VC removing towers 50A;First VC removing towers 50A is connected with the second serum mixing channel 48B, the mixing of the second serum Groove 48B is connected with the 2nd VC removing towers 50B.
Carried out in blowpit 42 from when pushing back receipts and negative pressure recovery, system can take the emulsifying agent and breast that foam includes out of Slurry, defoaming treatment is carried out via dynamic defoaming machine 41 and static Defoaming machine 40, this defoaming mode can not use defoamer It can complete, improve final product quality, be advantageous to downstream production, the serum that is captured is returned to after blowpit 42 again by thick wet type Pulverizer 43, thin wet crushing mill 44 and serum delivery pump 45 are delivered to after VC removing towers are removed and carried out into drying tower 53 Dry.
The VC contents of serum tentatively can be down to below 2000ppm by the step by 16000~20000ppm, reclaimed big The VC of amount, reduce VC unit consumption.
, VC recovery removing:
PVC serums in blowpit 42 are pumped in the first VC removing towers 50A by spray nozzle by serum conveying, make PVC Serum can be suitably distributed in tower wall, and temperature and vacuum in control tower.PVC breasts through first order removing tower 50A removings Slurry is from bottom of towe pipeline via being pumped into the 2nd VC removing towers 50B.Before second level removing tower is added, PVC serums pass through heating If reserve steam is heated to control temperature.After two-stage removes, the content of vinylchloride in serum is down to by about 2000ppm Below 300ppm.
After first VC removing towers are heated with steam, vapor (steam) temperature is controlled at 50~80 DEG C.Serum is in two level removing tower Residence time is 3~6 hours, after two level removes, content of vinylchloride in serum is down to 200 by 2000~2200ppm~ Below 300ppm.VC monomers have further been reclaimed, have reduced VC unit consumption, can have been made in follow-up drying process exhaust outlet emission VC contents are less than below 10ppm, and package unit will be more environmentally-friendly.Vacuum degree control scope in removing tower:- 400~-700mmH2O (About -0.004~-0.007Mpa).
, spray drying:
Serum after being reclaimed by the 2nd VC removing towers 50B enters in serum groove 51, and the serum in serum groove 51 enters again Enter in drying tower 53, dried resin sequentially enters pulverizer 54 into one section of bag hose 57, filter screen 56 and hopper 55 and carried out Crushed work, malleation discharge pressure control range is conveyed with malleation:3000-5000mmH2O(About 0.03~-0.05Mpa)To into Product feed bin 57, malleation fed distance can make the integral arrangement of dry, packaging and finished room more flexible, warp up to 200m or so Warehouse for finished product is sent into after automatic packaging system 60, automatic packaging system 60 uses open type or port type automatic packaging system.
, drying tower high pressure cleans automatically:
Drier is using the rinse water used in automatic high pressure cleaning equipment(It must be desalted water that rinse water, which refers to,)Stress control model Enclose:20~35Mpa;Spray dryer operation can be attached in tower wall through slurry after a period of time, can be dropped in producing Pollute paste resin finished product and influence quality, so Xu Let surely a period of time via automatic high pressure cleaning equipment can effectively by Tower wall cleans up;Rinse water Stress control model used in the automatic high pressure cleaning equipment of the automatic cleaning step of drying tower high pressure Enclose:20~35Mpa;The automatic cleaning step of drying tower high pressure, labor intensity can be greatly lowered, improve final product quality and finished product Rate.
, waste water continuously automatically processes:The continuous automated processing system of waste water is controlled by DCS, reduces labor intensity.
The wastewater collection discharged from latex groove 51, polymerization reaction kettle 36, blowpit 42, drying tower is in waste water collection tank 10 In, VC contents are in 3000~5000ppm in the waste water in waste water collection tank 10;Waste water reclaims in waste water after stripping and remains VC, VC contents are down to 100 below ppm;Waste water(COD contents 2000-3000ppm, SS content 3000-5000ppm)It is collected in waste water Equalization basin 6 is again through fast mixed groove 4 mixed slowly(Mixed 80~100 revs/min of revolution soon)Enter afterwards in neutralization chamber 3, enter again from neutralization chamber 3 It is floating except in groove 2, automatic scraping is except the sludge of concentration, sludge pumping to the automatic dehydration of the first centrifuge 8, dehydration to enter air Self-pressurizing agri Sold after collecting into mud cake packaging, floating to deliver to sand filtration tank 1 except rear waste water and automatically continuously handled, COD contents are down to 200ppm Hereinafter, then wastewater treatment center processing is delivered to.
The final products that the technique of the present invention is obtained, are applied to:Produce laminate adhesive agent, preventing stone hitting automobile chassis applies Layer, weave cotton cloth coating and required resin during substrate.
The bottom injection steam of waste water collection tank 10, injects from waste water pot bottom;The operating condition of steam:Temperature 80~98 DEG C, the mmHg of pressure -400~-700(About -0.004~-0.007Mpa).
The invention is not restricted to the data of each parameter value cited by above-described embodiment, as long as using the device of the present invention, and The technological process carried out by the device and the final products obtained, are accordingly to be regarded as within protection scope of the present invention.
The present invention can improve product quality, and chemical defoamer need not be added in removal process, and sewage can reach continuous Change is handled, and increases substantially production capacity, reduces labor intensity, reduces production cost.

Claims (9)

1. a kind of production technology for producing polyvinyl chloride interpolymer paste resin device, the device includes head tank, stripper, and seed is anti- Answer kettle, polymerization reaction kettle, gas holder, blowpit, drying tower, waste water collection tank, head tank and seed reactor and polymerization reaction kettle Connection, seed reactor are connected by seed storage tank with polymerization reaction kettle, and polymerization reaction kettle is connected with blowpit, and blowpit passes through Removing tower is connected with drying tower, and stripper, blowpit, seed reactor and polymerization reaction kettle are connected with gas holder respectively, gas holder with VCM recycling can connects, and seed reactor, polymerization reaction kettle, blowpit and drying tower connect with waste water collection tank respectively Connect, waste water collection tank is connected with stripper;Stripper is connected by equalization basin with measuring tank, and measuring tank connects with fast mixed groove mixed slowly Connecing, fast mixed groove mixed slowly is connected with neutralization chamber, and neutralization chamber is floating except groove is connected with sand filter and centrifuge respectively with floating except groove is connected, Sand filter is connected with treatment center of sewage;Head tank includes VAM tank, VCM tank, hot desalinized water tank, de- Brine tank, emulsifying agent tank, catalyst tank, initiator tank and buffer tank, aforementioned base materials tank is respectively with seed reactor and polymerizeing Reactor connects;The first automatic cleaning is provided with seed reactor and spraying mechanism and first concentrates charge pipe, polymerisation The second automatic cleaning and spraying mechanism and second are provided with kettle and concentrates charge pipe, polymerization reaction kettle is closed jacket structured;Unload Dynamic defoaming machine is housed, dynamic defoaming machine is connected with static Defoaming machine, and static Defoaming machine is connected with gas holder, static state defoaming on hopper The loop of machine is connected with blowpit;Blowpit passes sequentially through thick wet crushing mill, thin wet crushing mill, serum delivery pump and serum Mixing channel is connected with removing tower, and the Defoaming machine being connected with gas holder is provided with removing tower, and removing tower passes through latex groove and drying Tower connects, and drying tower passes sequentially through one section of bag hose, screen cloth, hopper, pulverizer, two sections of bag hoses and is connected with finished product bin;Kind Sub- reactor is connected by seed storage tank with polymerization reaction kettle;Anti-fouling agent tank and terminator tank are further equipped with device;
Its production technology is controlled by DCS, is carried out as follows:
, raw material prepare:
VCM of the VCM flask volume than 15% ~ 40% will be accounted for and add poly- seed reactor as charging for the first time In polymerization reaction kettle, VAM is added after polymerization reaction kettle has been fed in VCM and all added, and is participated in altogether Poly- reaction;Emulsifying agent, buffer, initiator are continuously added in seed reactor and polymerization reaction kettle, and catalyst disposably adds In seed reactor and polymerization reaction kettle;
, seed prepare
Hot desalinized water is added in seed reactor, and emulsifying agent is added when reacting and starting, and to form polyvinyl chloride particles, works as kind Sub- reactor pressure drops to 4 to 6Kg/cm2When, VCM is added, when seed reactor pressure drop, cooling valve close When closing, polyvinyl chloride particles enter seed storage tank;
, rear polymerization:
Hot desalinized water is delivered in polymerization reaction kettle, is in proportion added aforementioned particles in polymerization reaction kettle by seed;Vinyl acetate Monomer all adds when seed reactor and polymerization reaction kettle add VCM for the first time;Reaction pressure will polymerize Speed declines after slowing down, and shows that polymerization terminates;
, blowing recovery defoaming:
When the pressure in polymerization reaction kettle is down to 0. 02~0. 08Mpa, discharge of materials to blowpit is reclaimed and stored;Using Negative pressure reclaims, and when pressure is down to 0. 02~0. 08Mpa in blowpit, starts vavuum pump recovery, steam is passed through in blowpit Portion is heated up, and serum temperature reaches 40 DEG C~80 DEG C, and pressure reaches -400~-700mmH in blowpit2Terminate during O;
The negative pressure recovery stage of blowpit terminates, and serum is pumped into VC recovery defoamings from blowpit conveying;
Being carried out in blowpit from when pushing back receipts and negative pressure recovery, system can take the emulsifying agent and serum that foam includes out of, via Dynamic defoaming machine and static Defoaming machine carry out defoaming treatment, and the serum that is captured is pumped to drying system again after returning to blowpit It is dried;
, VC recovery removing:
PVC serums in blowpit are sent in removing tower by spray nozzle, and after removing tower is heated with steam, serum stops in removing tower Stay 3~6 hours, after removing, the content of vinylchloride in serum is down to 200~below 300ppm by 2000~2200ppm;
, spray drying:
Serum after being reclaimed by removing tower, which enters, to be dried in groove, and the serum dried in groove is entered back into drying tower, after drying Resin into bag hose collect, be sent into warehouse for finished product;
, drying tower high pressure cleans automatically:
Drier is using the rinse water pressure control range used in automatic high pressure cleaning equipment:20~35Mpa;
, waste water continuously automatically processes:
The wastewater collection discharged from latex groove, polymerization reaction kettle, blowpit, drying tower is in waste water collection tank, wastewater collection VC contents are in 3000-5000ppm in waste water in groove;Waste water reclaims in waste water after stripping and remains VC, VC contents are down to 100 Below ppm;Wastewater collection imports that air Self-pressurizing agri is floating to remove groove in waste water equalization basin after fast mixed slow mixed again, strikes off the dirt of concentration Mud, sludge pumping to centrifuge, it is dehydrated after collection is packed into mud cake to sell and floats except rear waste water delivers to sand filtration tank progress automatically continuously Processing, COD contents are down to below 200ppm, then deliver to wastewater treatment center processing.
2. the production technology of production polyvinyl chloride interpolymer paste resin device according to claim 1, it is characterised in that:Emulsification Agent is divided into two kinds, and wherein emulsifier EM 1 is used for polymerization prepared by emulsion seed, and with water dissolvable thing, company is pre-dissolved in emulsifying agent groove It is continuous to add in seed reactor;Emulsifier EM 2 is used for the preparation of emulsion chlorine vinegar interpolymer paste resin, is a kind of and water dissolvable thing, It is to be pre-dissolved to be continuously added in polymerization reaction kettle in emulsifying agent groove.
3. the production technology of production polyvinyl chloride interpolymer paste resin device according to claim 1, it is characterised in that:Catalysis Agent is divided into two classes, catalyst AC1, is the material with water soluble, and similar mode is pre-dissolved in catalyst tank, is to pass through gravity stream It is disposable to add in seed reactor;Catalyst AC2, be pre-dissolved with the material of water soluble in pre- fluid bowl, be by gravity stream once Property add reactor in.
4. the production technology of production polyvinyl chloride interpolymer paste resin device according to claim 1, it is characterised in that:Buffering Agent is divided into two kinds, is added to seed reactor and polymerization reaction kettle simultaneously after the mixing of both phosphoric acid and caustic soda, to ensure that pH exists 7~8。
5. the production technology of production polyvinyl chloride interpolymer paste resin device according to claim 1, it is characterised in that:Trigger Agent is divided into two kinds, and initiator CAT1 is prepared for seed, and it is a kind of and water dissolvable peroxide, is to trigger Agent tank, which is pre-dissolved, to be continuously added in seed reactor;Initiator CAT2 is prepared for emulsion chlorine vinegar interpolymer paste resin, and it is one Kind and the peroxide of water dissolvable, are to be pre-dissolved to be continuously added in polymerization reaction kettle in initiator tank.
6. the production technology of production polyvinyl chloride interpolymer paste resin device according to claim 1, it is characterised in that:Seed Reactor and polymerization reaction kettle are also connected with anti-fouling agent tank respectively, and anti-fouling agent is sprayed by 1.2 ~ 2.0Mpa steam jet ejectors Enter seed reactor and polymerization reaction kettle, fog is produced in kettle, make all inwalls of biologically active prod covering reactor.
7. the production technology of production polyvinyl chloride interpolymer paste resin device according to claim 1, it is characterised in that:Poly- Close under out-of-control condition, inject terminator terminating reaction process;Seed reactor and polymerization reaction kettle are respectively equipped with two terminations Agent tank, two terminator tanks are 1.6 ~ 2.5MPa nitrogen seal pressures.
8. the production technology of production polyvinyl chloride interpolymer paste resin device according to claim 1, it is characterised in that:Chloroethene Before alkene condensation, recovery vinyl chloride is handled with stabilizer and liquid caustic soda.
9. the production technology in a kind of claim 1 to 8 described in any one obtains the application of product:Sticked together for producing laminate Agent, preventing stone hitting automobile chassis coating, weave cotton cloth coating and required resin during substrate.
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