CN104437255A - Reaction kettle and method for producing ADC foaming agent by biurea oxide - Google Patents

Reaction kettle and method for producing ADC foaming agent by biurea oxide Download PDF

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Publication number
CN104437255A
CN104437255A CN201410661382.2A CN201410661382A CN104437255A CN 104437255 A CN104437255 A CN 104437255A CN 201410661382 A CN201410661382 A CN 201410661382A CN 104437255 A CN104437255 A CN 104437255A
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China
Prior art keywords
biruea
still
chlorine
kettle
reactor
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CN201410661382.2A
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CN104437255B (en
Inventor
汪国清
汪新泉
王寿发
潘英曙
敖永平
丁浩
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JIANGXI SELON INDUSTRIAL Co Ltd
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JIANGXI SELON INDUSTRIAL Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/04—Pressure vessels, e.g. autoclaves
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C281/00—Derivatives of carbonic acid containing functional groups covered by groups C07C269/00 - C07C279/00 in which at least one nitrogen atom of these functional groups is further bound to another nitrogen atom not being part of a nitro or nitroso group
    • C07C281/20—Derivatives of carbonic acid containing functional groups covered by groups C07C269/00 - C07C279/00 in which at least one nitrogen atom of these functional groups is further bound to another nitrogen atom not being part of a nitro or nitroso group the two nitrogen atoms of the functional groups being doubly-bound to each other, e.g. azoformamide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00002—Chemical plants
    • B01J2219/00004—Scale aspects
    • B01J2219/00006—Large-scale industrial plants
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00054—Controlling or regulating the heat exchange system
    • B01J2219/00056—Controlling or regulating the heat exchange system involving measured parameters
    • B01J2219/00058—Temperature measurement
    • B01J2219/00063—Temperature measurement of the reactants
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00054—Controlling or regulating the heat exchange system
    • B01J2219/00056—Controlling or regulating the heat exchange system involving measured parameters
    • B01J2219/00069—Flow rate measurement
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00761—Details of the reactor

Abstract

The invention relates to a reaction kettle and a method for producing an ADC foaming agent by biurea oxide, and a detection method for quality control after reaction is finished. The area and the quantity of cooling assemblies in the kettle can be set according to requirements; the plurality of groups of parallel cooling assemblies are arranged in the kettle; and a DCS is used so that the reaction temperature and the chlorine filling amount in the kettle are accurately controlled, and large output and high yield of the ADC foaming agent are realized. Meanwhile, a measuring method for biurea particle residues at the reaction tail end is adopted so that the high yield is realized again. The product with high yield and good quality is obtained in the reaction kettle with the size being 30m<3>-50m<3>.

Description

A kind of reactor and method being oxidized biruea production ADC blowing agent
Technical field
The present invention relates to ADC blowing agent field, be specifically related to a kind of reactor and the method that are oxidized biruea production ADC blowing agent.
Background technology
Blowing agent can in very narrow temperature range for Celogen Az (being called for short ADC), decompose in the extremely short time and produce a large amount of gas, and the gas generated and residue is nontoxic, odorless, pollution-free, not painted, not corrode processing equipment, the mechanical property not affecting goods and stability, good dispersiveness is had in plastics and rubber, the abscess formed is evenly fine and closely woven, is the organic foaming agent that range of application is the widest in the world.
ADC blowing agent is mainly made by oxidation biruea, and wherein chlorine oxidation process is because its cost is low, and technical maturity, raw material are easy to get, simple operation and other advantages, apply comparatively general.Adopt the method oxidation biruea of chlorin distributer under a cauldron in Chinese patent application 103193685, achieve domain size distribution and the good ADC blowing agent of gas forming amount, but also just a small amount of reaction.Usually in, large quantitative response is in the employing of oxidizing reactor, adopts chuck enamel still, and on enamel still, carry out the carbon steel still that improves, titanium coil pipe is inside established to cool, though this kind of reactor heat-transfer effect is better than enamel still, its volume also can be accomplished comparatively large, reaches 20-22m 3.
DCS is the english abbreviation (Distributed Control System) of dcs, is the product that computer technology, control technology and network technology height combine.DCS adopts several controllers (process station) to control the numerous control points in a production process usually, is connected and can carry out exchanges data between each controller by network.In chemical process, use DCS control system, improve in production process the efficiency operating, manage, monitor.And by using the method for decentralised control to control art production process, not only reduce the fussy degree of operator's work, and make the security of production higher.
Summary of the invention
First technical problem that the present invention solves is to provide a kind of reactor producing ADC blowing agent for being oxidized biruea, comprise reactor and comprise kettle 4, kettle cover 2, be built in cooling device 3 in the still in kettle, be arranged on the stirring motor 1 on kettle cover, stirring motor is connected with corrosion-resistant composite agitator, kettle has and fills chlorine mouth 5 and still outlet valve 6, kettle cover comprises charging aperture, wherein in still, cooling device has many cooling tubes, the area of cooling package and quantity can be arranged as required.Because chilling temperature can by the use amount of controlled cooling model device, reactor volume can accomplish 30-50 cubic meter.Often organize cooling device in still and be arranged in parallel turnover two adapter, be mainly used in the turnover of cooling water, wherein in still, cooling device is 6-8 group.
Second technical problem that the present invention solves is to provide a kind of method of producing ADC blowing agent for being oxidized biruea, DCS system is used to carry out control aforesaid reaction vessel, comprise the following steps: 5-10 ton biruea passes in reactor according to claim 1 by (1), adds a certain amount of auxiliary agent; (2) controlling pressure in still by DCS system is tiny structure, and vacuum is-30/-50mmHg; (3) open chlorine valve, chlorine is filled with in still from stills for air blowing bottom valve, fills chlorine dose and controls at 50-300m 3temperature in the kettle, by the control to chilled water unit, controls between 38-42 DEG C by/h reactor; (4), when in still, pressure transfers malleation to from tiny structure, stop passing into chlorine.
In order to ensure the productive rate of ADC blowing agent, the 3rd technical problem that the present invention solves is the use of a kind of inspection
The method of the ADC blowing agent quality obtained after oxygen determination, step is as follows, (1) when in the still described in claim 7, malleation transfers negative pressure again to, a peek 100mL feed samples is in beaker, repeatedly most to ADC rinsing with water rinse, the cup end, is without biruea particle residue, or biruea remains in less than 2, and reaction terminates.(2) if biruea at the bottom of cup is residual be greater than 2, be then considered as biruea particle and exceed standard, continue logical chlorine in stills for air blowing, control again to fill chlorine dose according to biruea particle residue quantity, to still, pressure transfers malleation to, stops logical chlorine.
Present invention produces following technique effect:
1., owing to adopting oxidizing reactor of the present invention, supporting cooling device structure equilibrium and interior hot side are long-pending large, can fully regulate stills for air blowing interior reaction temperature, so stills for air blowing volume can greatly to 30-50m 3, formed and produce in a large number, drastically increase the efficiency of reaction.
2. pass into the control of chlorine and amount of chlorine at the bottom of still, chlorine is fully contacted with material, and chlorine utilization improves 6-8%.
3. adopt DCS system to control the reactor of the present invention's design, accurate control reaction temperature, improve the stability of reaction, reaction completion rate is made to be close to 100%, compared to using detection method before, biruea particle residue will fill chlorine reaction through 2-4 time just can obtain qualified products, has had very much progress.
4., after reaction terminates, the measuring method of biruea particle residue, ensure that the realization of high yield.
5., with reclaiming oxidation mother liquor washings dissolved oxygen auxiliary agent, oxidation promoter consumption only has original 1/3rd more than.
accompanying drawing explanation
Fig. 1 is the reactor that oxidation biruea produces ADC blowing agent
1. stirring motor 2. kettle cover 3. cooling device 4. kettle 5. chlorinator 6. still outlet valve
Fig. 2 is the stereogram of oxidizing reactor bottom stirrer.
Detailed description of the invention
embodiment 1
Reaction starts, and uses 30m 2oxidizing reactor, in still, cooling device quantity is 6 groups.Controlled by DCS system, throw in biruea 5.2 tons, be dissolved in by 20kg auxiliary agent in oxidation mother liquor dissolving and drop in stills for air blowing, auxiliary agent is usual auxiliaries.Control to keep tiny structure, vacuum-30 ~-50mmHg in still.Start to fill chlorine, fill chlorine dose and control at 80-180m 3/ h, reaction temperature controls between 38-42 DEG C, and system can regulate the quantity of the cooling device of the cooling water passed into automatically according to temperature in the kettle.
When in still, pressure transfers malleation to, stop passing into chlorine, get three 100mL feed samples respectively in 500mL beaker, repeatedly most to ADC rinsing with water rinse, all without biruea particle residue at the bottom of three cups, reaction terminates, wash, disposing mother liquor utilizes, and solid ADC blowing agent is finished product through centrifugal, drying, obtain 5.14 tons of ADC blowing agents, gas forming amount 235.6 mL/g.
If biruea at the bottom of cup is residual be greater than 2, is then considered as biruea particle and exceeds standard, continue logical chlorine in stills for air blowing, control again to fill chlorine dose according to biruea particle residue quantity, to still, pressure transfers malleation to, stops logical chlorine.
Adopt said method, duplication of production tests 100 times, and it is zero that reaction terminates the biruea particle number of times that exceeds standard, and every still output is all more than 4.90 tons, and gas forming amount is between 230 ~ 240 mL/g.
embodiment 2
Reaction starts, and uses 50m 2in oxidizing reactor, in still, cooling device quantity is 8 groups.Controlled by DCS system, throw in biruea 8.4 tons, be dissolved in by 30kg auxiliary agent in oxidation mother liquor dissolving and drop in stills for air blowing, auxiliary agent is usual auxiliaries.Control to keep tiny structure, vacuum-30 ~-50mmHg in still.Start to fill chlorine, fill chlorine dose and control at 150-300m 3/ h, reaction temperature controls between 38-42 DEG C, and system can regulate the quantity of the cooling device of the cooling water passed into automatically according to temperature in the kettle.
When in still, pressure transfers malleation to, stop passing into chlorine, get three 100mL feed samples respectively in 500mL beaker, repeatedly most to ADC rinsing with water rinse, without biruea particle residue at the bottom of a cup, biruea particle residue 1 at the bottom of two cups, reaction terminates, and washs, disposing mother liquor utilizes, solid ADC blowing agent is finished product through centrifugal, drying, obtains 8.09 tons of ADC blowing agents, gas forming amount 238 mL/g.
Adopt said method, duplication of production tests 100 times, and reaction terminates the biruea particle number of times that exceeds standard and is only 1 time.After biruea particle exceeds standard, transfer tiny structure to, pass into chlorine in still to be oxidized, to still, pressure stops after transferring malleation to, again detects, and biruea particle residue is qualified.
Obtain every still output thus all more than 8 tons, gas forming amount is between 230 ~ 240 mL/g.
Embodiment 3
Fig. 2 can be arranged on the agitator bottom oxidizing reactor, stirrer bottom with fill chlorine hole and be connected, whip topping is provided with an opening, opening is slightly less than into chlorine hole, be provided with the ridge with agitating function at the back of agitator simultaneously, crestal culmination end is for opening rear design, after reaction starts, feed liquid is rotated along with the stirring of upper agitator, bottom stirrer rotates along with feed liquid, pass into gas simultaneously, for fully mixing of feed liquid and gas, promote homogeneous reaction, also agitator can be connected with motor, stir with upper agitator rightabout, promote the abundant stirring of feed liquid, make the product quality after oxidation more even.

Claims (8)

1. one kind is oxidized the reactor that biruea produces ADC blowing agent, employing DCS system controls, comprise kettle (4), kettle cover (2), be built in cooling device (3) in the still in kettle, be arranged on the stirring motor (1) on kettle cover, stirring motor is connected with corrosion-resistant composite agitator, kettle has and fills chlorine (5) and still outlet valve (6), kettle cover comprises charging aperture, it is characterized by: cooling device has many cooling tubes in still, the area of cooling package and quantity can be arranged as required.
2. reactor according to claim 1, is characterized by: described reactor volume is 30-50 cubic meter.
3. reactor according to claim 1, is characterized by: often organize cooling device in described still and be arranged in parallel turnover two adapter.
4. reactor according to claim 3, is characterized by: the turnover being used for cooling water is taken in described turnover two.
5. the arbitrary claim according to right 1 to 4, is characterized by: in still, cooling device is 6-8 group.
6. DCS system controls the method that a large amount of oxidation biruea produces ADC blowing agent, it is characterized in that: use the reactor described in claim 1 to react.
7. oxidation biruea according to claim 6 produces the method for ADC blowing agent, it is characterized in that: comprise the following steps: 5-10 ton biruea passes in reactor according to claim 1 by (1), adds a certain amount of auxiliary agent; (2) controlling pressure in still by DCS system is tiny structure, and vacuum is-30/-50mmHg; (3) open chlorine valve, chlorine is filled with in still from stills for air blowing bottom valve, fills chlorine dose and controls at 50-300m 3temperature in the kettle, by the control to chilled water unit, controls between 38-42 DEG C by/h reactor; (4), when in still, pressure transfers malleation to from tiny structure, stop passing into chlorine.
8. oxidation biruea according to claim 7 produces the method for ADC blowing agent, it is characterized in that: the method step for the ADC blowing agent quality obtained after detecting oxidation comprises: when (1) malleation transfers negative pressure again in the still described in claim 7, get 100mL feed liquid in beaker, repeatedly most to ADC rinsing with water rinse, the cup end, is without biruea particle residue, or biruea remains in less than 2, reaction terminates, (2) if biruea at the bottom of cup is residual be greater than 2, then be considered as biruea particle to exceed standard, stills for air blowing continue logical chlorine, control again to fill chlorine dose according to biruea particle residue quantity, to still, pressure transfers malleation to, stop logical chlorine.
CN201410661382.2A 2014-11-19 2014-11-19 A kind of reactor aoxidizing biruea production ADC foaming agent and method Active CN104437255B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104817478A (en) * 2015-04-15 2015-08-05 江苏索普（集团）有限公司 Method for recovering biurea and preparing azodicarbonamide
CN113262747A (en) * 2021-06-21 2021-08-17 宿迁苏博科技信息有限公司 Production process and equipment of special foaming accelerant for rubber

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102675158A (en) * 2012-05-10 2012-09-19 杭州海虹精细化工有限公司 Method for producing ADC foaming agent by using chlorine gas-oxidized HDCA (biurea) in saturated hydrochloric acid solution
CN103012218A (en) * 2012-12-14 2013-04-03 杭州海虹精细化工有限公司 Method of semi-continuously producing particle-size-controllable ADC (azodicarbonamide) foaming agent
CN103193685A (en) * 2013-03-28 2013-07-10 杭州海虹精细化工有限公司 Method for producing ADC (azodicarbonamide) foaming agent by chlorine dioxide biurea
CN103657574A (en) * 2013-11-27 2014-03-26 杭州海虹精细化工有限公司 Device for preparing ADC (azodicarbonamide) foaming agent by self-suction oxidation

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102675158A (en) * 2012-05-10 2012-09-19 杭州海虹精细化工有限公司 Method for producing ADC foaming agent by using chlorine gas-oxidized HDCA (biurea) in saturated hydrochloric acid solution
CN103012218A (en) * 2012-12-14 2013-04-03 杭州海虹精细化工有限公司 Method of semi-continuously producing particle-size-controllable ADC (azodicarbonamide) foaming agent
CN103193685A (en) * 2013-03-28 2013-07-10 杭州海虹精细化工有限公司 Method for producing ADC (azodicarbonamide) foaming agent by chlorine dioxide biurea
CN103657574A (en) * 2013-11-27 2014-03-26 杭州海虹精细化工有限公司 Device for preparing ADC (azodicarbonamide) foaming agent by self-suction oxidation

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104817478A (en) * 2015-04-15 2015-08-05 江苏索普（集团）有限公司 Method for recovering biurea and preparing azodicarbonamide
CN113262747A (en) * 2021-06-21 2021-08-17 宿迁苏博科技信息有限公司 Production process and equipment of special foaming accelerant for rubber

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