CN102964341A - Production system of triglycidyl isocyanurate - Google Patents
Production system of triglycidyl isocyanurate Download PDFInfo
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- CN102964341A CN102964341A CN2012104947001A CN201210494700A CN102964341A CN 102964341 A CN102964341 A CN 102964341A CN 2012104947001 A CN2012104947001 A CN 2012104947001A CN 201210494700 A CN201210494700 A CN 201210494700A CN 102964341 A CN102964341 A CN 102964341A
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Abstract
The invention discloses a production system of triglycidyl isocyanurate. The production system comprises a filtering device, a drying device and a heat collecting unit, wherein the filtering device is used for filtering a mixture produced by the reaction in a cyclization reaction kettle; the drying device is used for heating the residual solid salt waste generated in the filtering process of the filtering device; the heat collecting unit is used for collecting the heat generated by the reaction in a synthetic reaction kettle; and the heat collecting unit is connected with a heating unit by a pipeline, wherein the heating unit is arranged on the drying device and is used for heating the solid salt waste. According to the production system of the triglycidyl isocyanurate, the heat generated by the reaction in the synthetic reaction kettle is collected and used for heating the solid salt waste, so that the organic matter and moisture in the solid salt waste can be heated to be evaporated, and the salt and other components in the solid salt waste can be separated and then recycled respectively, and as a result, the effective treatment of the solid salt waste can be realized; and the afterheat produced in the production can be comprehensively utilized, so that the cost of processing the solid salt can be reduced.
Description
Technical field
The present invention relates to the isocyanuric acid three-glycidyl ester production field, be specifically related to a kind of production system of isocyanuric acid three-glycidyl ester.
Background technology
Isocyanuric acid three-glycidyl ester (TGIC) is a kind of neo-epoxy resin, has good thermotolerance, weathering resistance, cohesiveness and electrical properties in high temperatures, and is high to acid, alkali and other chemical stability, has good especially crosslinking curing performance.Be to contain one of most important solidifying agent of carboxyl functional group base-material, be particularly useful for the solidifying agent of powder coating carboxy(l)polyester.
The production technique that TGIC generally uses as shown in Figure 1, being about to epoxy chloropropane (ECH), cyanuric acid (CA) adds according to a certain ratio with an amount of catalyzer and carries out building-up reactions in the reactor, obtain intermediate product 1,3,5-three (1 '-chloro-2 '-hydroxyl-propyl) chlorinated isocyanurates, again intermediate product and solid sodium hydroxide generation cyclization are obtained containing the mixture of TGIC, this mixture after filtration, can make the TGIC finished product after the operation such as distillation, crystallization, oven dry.Although this technique can effectively be produced the TGIC finished product, it can produce a large amount of solid salt refuses in process of production, and the complicated component of these solid salt refuses comprises NaCl, ECH, H
2The Multiple components such as O, especially ECH are poisonous volatile substances, as directly toppling over or landfill, will inevitably destroy ecotope, contaminated soil.Therefore, how to process for a long time solid salt refuse and become the technical barrier that TGIC produces.
At present, the scheme that solid salt refuse is processed of having reported mainly adopts burning disposal or organic solvent extraction to process, wherein scheme is preferably: name is called " research of TGIC process for cleanly preparing ", Feng Deli, Deng. Speciality Petrochemicals progress .2007,8 (1): disclosed employing adds the ECH that suction filtration is removed in the solid salt refuse behind the methanol extraction and makes industrial salt (seeing its open file Fig. 1 for details) in the document of 56-58, although the method can effectively be removed the ECH organism in the solid salt refuse, but the NaCl rate of recovery is low, Gu because also contain the moisture that contains in part moisture and the methyl alcohol in the salt refuse, therefore meeting is difficult to reclaim so that part NaCl is soluble in water.In addition, along with the reuse number of times raising of extracting mother liquid, produce the salt rate and also descending.Simultaneously, be worth not highly from industrialization angle Industrial Salt itself, the cost of methyl alcohol or alcohol extraction technique is high, operate comparatively loaded down with trivial detailsly, so is difficult to carry out industrial applications.
Summary of the invention
The production system that the purpose of this invention is to provide a kind of isocyanuric acid three-glycidyl ester is processed the solid salt refuse that produces in producing, and improves the economic benefit that TGIC produces, save energy.
A kind of production system of isocyanuric acid three-glycidyl ester, comprise the filtration unit that filters for the mixture after cyclization still internal reaction is finished, it is characterized in that: this production system also comprise filtration unit filtered after remaining solid salt refuse carry out the drying installation of heat treated and liberated heat is collected when reacting in the synthesis reaction vessel thermal-arrest unit, this thermal-arrest unit is connected by the heating unit that adds thermosetting salt refuse that arranges on pipeline and the drying installation.
Among the application, collect be used to adding thermosetting salt refuse by liberated heat when reacting in the synthesis reaction vessel, so that organism and moisture in the solid salt refuse are subjected to thermal evaporation, thereby so that the salinity in the solid salt refuse is separated with other components, and then utilize respectively, thereby solid salt refuse is effectively processed.Simultaneously the waste heat that produces in producing is fully utilized, reduce the cost that solid salt is processed.
Description of drawings
Fig. 1 is the traditional production technological process of TGIC;
Fig. 2 is structural representation of the present invention.
Embodiment
The application's purpose is to provide a kind of production system of isocyanuric acid three-glycidyl ester, says accurately the production system for a kind of isocyanuric acid three-glycidyl ester that can effectively process the solid salt refuse that produces in producing.So far solid salt refuse can not get effective processing during TGIC produced, its reason mainly contain following some: produce to produce the organic species number and the number change that contain in the solid salt refuse larger for each batch in the first TGIC production process, therefore the salt refuse is not a stable mixture that forms admittedly, therefore can not directly use as product or raw material; It two is also not find in the prior art to carry out that effective separation reclaims and to the approach that each component that reclaims is effectively utilized to solid salt refuse, therefore mostly adopts to burn or calcining is processed.The scheme that adopts among the application, as shown in Figure 2, a kind of production system of isocyanuric acid three-glycidyl ester, comprise the filtration unit 13 that filters for the mixture after cyclization still 12 internal reactions are finished, this production system also comprise filtration unit 13 filtered after remaining solid salt refuse carry out the drying installation 14 of heat treated and liberated heat is collected when reacting in the synthesis reaction vessel 11 thermal-arrest unit 20, this thermal-arrest unit 20 is connected by the heating unit that adds thermosetting salt refuse of setting on pipeline and the drying installation 14.Like this by solid salt refuse being carried out heat treated in that drying installation 14 is interior, evaporation separates so that the organic phase in the solid salt refuse is with moisture, thereby obtain the extremely low dried salt of volatile content, because dried salt volatile content is extremely low, therefore can be with its raw materials for production as frostproofer for building or raising agent, and the organism of separating can be again as the raw material of building-up reactions.Among the application, by the solid salt refuse in producing is processed recycling, and the waste heat that building-up reactions in producing is produced fully utilizes, thereby realizes cleaner production and the energy-saving and emission-reduction of TGIC.Because the difference of production technique, the operation that may produce solid salt refuse respectively is not quite similar, the issuable solid salt refuse of other operations can certainly be inserted in the drying installation and process, in this application, in filtration unit 13, carry out the crystallization filtration treatment by the mixture that obtains after cyclization still 12 internal reactions are finished, obtain solid phase and be solid waste (wet salt) among the application, so that cyclization obtains moisture and the complete crystallization of salinity in the mixed system, filter the solid phase obtain by 82～83% NaCl by the crystallization filtration, ECH about 4%, H about 12%
2The catalyst combination of O and trace consists of, and obtains then not containing in the liquid phase or containing salt hardly and moisture, so that salinity, moisture separate fully with TGIC, byproduct of reaction, just can not produce solid salt refuse in other operation sequences like this.Simultaneously, the present invention adopts the method for physical sepn that solid salt refuse is processed, and produces the salt rate and can reach more than 80%, need consider the variation of its component concentration when avoiding solid salt waste chemistry to process and need to add auxiliary component, be easier to realize suitability for industrialized production, improve the economic benefit that TGIC produces.
Concrete scheme is that escaping gas carried out the organism recovery unit 30 that condensation is reclaimed when this production system also comprised heat treated.Described organism recovery unit 30 comprises drying installation 14 interior escaping gas is carried out the condenser of condensation and the liquid trap that the liquid of condensation is reclaimed.This production system also comprises the vacuum pump 33 that drying installation 14 is vacuumized, described drying installation 14 air outlets connect the first condenser 31, the first condenser 31 liquid flowing outlets are connected with main liquid trap 32, the inlet pipe of vacuum pump 33 is connected with main liquid trap 32 intracavity inter-connections, the vapor pipe of vacuum pump 33 is connected with the second condenser 34 inlet mouths and is connected, and the liquid flowing outlet of the second condenser 34 is connected with secondary liquid trap 35.The liquid that described major and minor liquid trap 32,35 is collected are delivered to respectively tripping device 36 to carry out component and separates, and separates to obtain organic phase and be delivered to that synthesis reaction vessel 11 is interior to participate in reaction again as raw material.The gas (that is organism and moisture of volatilization) that produces during 30 pairs of heat treated of organism recovery unit by arranging carries out recycling, because the hot water of liquid state that adopt as heat-conducting fluid more when actually operating, temperature when solid salt refuse is carried out heat treated can't be higher like this, therefore, for guaranteeing that the organism in the solid salt refuse can be steamed recovery fully, adopt among the application 33 pairs of drying installations of vacuum pump are vacuumized.Be provided with condenser and liquid trap on the inlet and outlet pipeline of vacuum pump 13 in this application, its purpose guarantees that first organism is by fully evaporative condenser recovery, second, because during heat treated, evaporation escaping gas amount is larger, by most of gas is collected in the 31 interior condensations of the first condenser and by main liquid trap 32, the gas volume that enters like this vacuum pump 33 reduces greatly, thereby by the vacuum pump 33 of less rate of air sucked in required is set, just can satisfy the requirement that drying installation 14 is vacuumized, reduce the equipment cost of whole system.If the vacuum pump 33 of larger rate of air sucked in required is set certainly here, also can cancel the setting of the first condenser 31 and main liquid trap 32, the secondary liquid trap 35 here can directly be made of a water tank.
For guaranteeing the smoothness running of whole production system, thermal-arrest unit 20 described in the application combines for first cavity for holding heat-conducting fluid of synthesis reaction vessel 11 perisporiums and/or inner setting, described the first cavity is connected with the heat storage can 22 that is used for the storage heat-conducting fluid by rising pipe 21 and is connected, described heating unit is that drying installation 14 perisporiums and/or inner the second cavity for holding heat-conducting fluid that arranges combine, described the second cavity is by connecting tube 23,24 and the pump housing 25 consist of the circulation path that heat-conducting fluids circulate with heat storage can 22, that is, the water inlet of heat storage can 22 water outlets by the second cavity on connecting tube 23 and the drying installation 14 is connected and is connected, the water outlet of the second cavity on the drying installation 14 is connected with heat storage can 22 water-ins by connecting tube 24 and is connected, and the pump housing 25 is set on the connecting tube 24.First and second cavity here can be used for holding hot-fluid by the sandwich structure that arranges on synthesis reaction vessel 11 and drying installation 14 perisporiums.Because required heat when liberated heat is greater than solid salt refuse heat treated during the synthesis reaction vessel internal reaction, therefore be provided with heat storage can 22 among the application, with heat storage can 22 and heating unit by connecting tube 23,24 and the pump housing 25 consist of a little water circulation path, thereby solid salt refuse is carried out effective heat treated, and the unnecessary heat of heat storage can 22 interior storages also can be utilized by other operations like this.Certainly, also can adopt directly first and second cavity is is directly connected and composed water circulation path by pipeline, but the utilization ratio of the waste heat that whole like this building-up reactions is emitted is lower.
Further, applicant's test of long duration finds that temperature and the vacuum tightness on solid salt refuse heat treated is larger on the impact of producing the salt rate in this system, therefore the applicant is by constantly revising technical scheme, final determine that the temperature of heat treated is 80～95 ℃, the vacuum tightness that drying installation 14 vacuumizes is-0.08～-0.094Mpa.Described drying installation 14 is rake type drier.Under this condition, Gu the product salt rate that the salt refuse is processed and the organism rate of recovery can improve 2～4 percentage points with respect to the technical scheme that realizes other parameters of the object of the invention.
When concrete operations, mixtures in the cyclization still 12 are placed carry out crystallization in the filtration unit 13 and filter, the wet salt (namely consolidating the salt refuse) that obtains is placed in the rake type drier, be provided with stirring mechanism in the rake type drier, dryer cavity is bilayer structure, can lead to hot water in the interlayer, combination of lumens becomes the second cavity, start vacuum pump 33 and first, two condensers 31,34 pairs of rake type driers vacuumize, when vacuum tightness reaches-0.08Mpa, open the inlet valve that arranges on the rake type drier, thereby the wet salt in the rake type drier is heated, wet salt is heated gradually and heats up, organism and moisture constantly in the material evaporation overflow and enter first, two condensers 31,34 and main, secondary liquid trap 32, collection is condensed in 35, after heat treated after a while, organic constituent in the wet salt and moisture are evaporated complete, namely obtain industrial dried salt (moisture below 3%), close the inlet valve and the vacuum pump 33 that arrange on the rake type drier, take out the raw materials for production that the interior dried salt of rake type drier namely can be used as frostproofer for building and raising agent.The liquid of collecting in the major and minor liquid trap 32,35 inserted carry out standing demix in the tripping device 36, then the organic phase of separating is dropped in the synthesis reaction vessel 11 again and react, the water of separation can be used as again water of productive use.
At present, process dried salt that solid salt refuse obtains to detect through Anhui Province's product quality supervision and testing institute by aforesaid operations, all technical meets the index request of company standard " frostproofer Q/DQS002-20082 " and " cement raising agent Q/DQS004-2008 ".End in August, 2012, industry accumulative total in bright and beautiful peak reclaims 120 batches in solid salt refuse, reclaims altogether more than 80 tons of dried salt, the ECH3.6 ton, and accumulative total reduces 85 tons of solid waste dischargings, is more than 90,000 yuan of enterprise's additional incomes.
The present invention can effectively realize solid salt refuse in the isocyanuric acid three-glycidyl ester production is processed in a word, waste heat to the solid salt refuse in the TGIC production and reaction generation carries out recycling, realize cleaner production, production energy-saving and green production, improve the economic benefit that TGIC produces.
Claims (8)
1. the production system of an isocyanuric acid three-glycidyl ester, comprise the filtration unit (13) that filters for the mixture after cyclization still (12) internal reaction is finished, it is characterized in that: this production system also comprise filtration unit (13) filtered after remaining solid salt refuse carry out the drying installation (14) of heat treated and liberated heat is collected when reacting in the synthesis reaction vessel (11) thermal-arrest unit (20), this thermal-arrest unit (20) is connected by the heating unit that adds thermosetting salt refuse of pipeline with the upper setting of drying installation (14).
2. the production system of isocyanuric acid three-glycidyl ester as claimed in claim 1 is characterized in that: escaping gas carried out the organism recovery unit (30) that condensation is reclaimed when this production system also comprised heat treated.
3. the production system of isocyanuric acid three-glycidyl ester as claimed in claim 1, it is characterized in that: described thermal-arrest unit (20) combines for first cavity for holding heat-conducting fluid of synthesis reaction vessel (11) perisporium and/or inner setting, described the first cavity is connected with the heat storage can (22) that is used for the storage heat-conducting fluid by rising pipe (21) and is connected, described heating unit is that drying installation (14) perisporium and/or inner the second cavity for holding heat-conducting fluid that arranges combine, and described the second cavity is by connecting tube (23,24) and the pump housing (25) and heat storage can (22) consist of the circulation path that heat-conducting fluid circulates.
4. the production system of isocyanuric acid three-glycidyl ester as claimed in claim 2 is characterized in that: described organism recovery unit (30) comprises the interior escaping gas of drying installation (14) is carried out the condenser of condensation and the liquid trap that the liquid of condensation is reclaimed.
5. the production system of isocyanuric acid three-glycidyl ester as claimed in claim 4, it is characterized in that: this production system also comprises the vacuum pump (33) that drying installation (14) is vacuumized, described drying installation (14) air outlet connects the first condenser (31), the first condenser (31) liquid flowing outlet is connected with main liquid trap (32), the inlet pipe of vacuum pump (33) is connected with main liquid trap (32) intracavity inter-connection, the vapor pipe of vacuum pump (33) is connected with the second condenser (34) inlet mouth and is connected, and the liquid flowing outlet of the second condenser (34) is connected with secondary liquid trap (35).
6. the production system of isocyanuric acid three-glycidyl ester as claimed in claim 5, it is characterized in that: the liquid that described major and minor liquid trap (32,35) is collected is delivered to respectively tripping device (36) to carry out component and separates, and separates to obtain organic phase and be delivered in the synthesis reaction vessel (11) and again participate in reaction as raw material.
7. the production system of isocyanuric acid three-glycidyl ester as claimed in claim 5, it is characterized in that: the temperature of described heat treated is 80～95 ℃, the vacuum tightness that drying installation (14) vacuumizes is-0.08～-0.094Mpa.
8. the production system of isocyanuric acid three-glycidyl ester as claimed in claim 6, it is characterized in that: described drying installation (14) is rake type drier.
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| CN201210494700.1A CN102964341B (en) | 2012-11-28 | 2012-11-28 | The production system of isocyanuric acid three-glycidyl ester |
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| CN201210494700.1A CN102964341B (en) | 2012-11-28 | 2012-11-28 | The production system of isocyanuric acid three-glycidyl ester |
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Cited By (3)
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|---|---|---|---|---|
| CN104327058A (en) * | 2014-08-07 | 2015-02-04 | 黄山锦峰实业有限公司 | Preparation method of 1,3,5-triglycidyl isocyanurate |
| CN113307802A (en) * | 2021-06-10 | 2021-08-27 | 黄山友谊南海新材料有限公司 | Processing method of high-purity triglycidyl isocyanurate |
| CN114130303A (en) * | 2021-11-27 | 2022-03-04 | 南京创博机械设备有限公司 | TGIC high-efficiency devolatilization and melt extrusion granulation integrated processing method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104327058A (en) * | 2014-08-07 | 2015-02-04 | 黄山锦峰实业有限公司 | Preparation method of 1,3,5-triglycidyl isocyanurate |
| CN104327058B (en) * | 2014-08-07 | 2017-08-25 | 黄山锦峰实业有限公司 | The preparation method of isocyanuric acid three-glycidyl ester |
| CN113307802A (en) * | 2021-06-10 | 2021-08-27 | 黄山友谊南海新材料有限公司 | Processing method of high-purity triglycidyl isocyanurate |
| CN113307802B (en) * | 2021-06-10 | 2023-10-27 | 黄山友谊南海新材料有限公司 | Processing method of high-purity triglycidyl isocyanurate |
| CN114130303A (en) * | 2021-11-27 | 2022-03-04 | 南京创博机械设备有限公司 | TGIC high-efficiency devolatilization and melt extrusion granulation integrated processing method |
| CN114130303B (en) * | 2021-11-27 | 2023-11-14 | 南京创博机械设备有限公司 | TGIC efficient devolatilization and melt extrusion granulation integrated processing method |
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