CN202989024U - Production system of isocyanuric acid tri-glycidyl ester - Google Patents

Production system of isocyanuric acid tri-glycidyl ester Download PDF

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Publication number
CN202989024U
CN202989024U CN 201220639967 CN201220639967U CN202989024U CN 202989024 U CN202989024 U CN 202989024U CN 201220639967 CN201220639967 CN 201220639967 CN 201220639967 U CN201220639967 U CN 201220639967U CN 202989024 U CN202989024 U CN 202989024U
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China
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production system
heat
isocyanuric acid
glycidyl ester
solid salt
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Expired - Fee Related
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CN 201220639967
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Chinese (zh)
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洪昭雷
王建坤
汪仁伟
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HUANGSHAN JINFENG INDUSTRIAL Co Ltd
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HUANGSHAN JINFENG INDUSTRIAL Co Ltd
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Abstract

The utility model discloses a production system of isocyanuric acid tri-glycidyl ester. The production system of the isocyanuric acid tri-glycidyl ester comprises a filter device, and further comprises a drying device and a heat collecting unit. The filter device is used for filtering a mixture after a reaction is finished in a cyclization reaction still. The drying device is used for carrying out heating processing on residual solid salt waste after filtration of the filter device. The heat collecting unit is used for collecting heat released by a reaction in a synthetic reaction still when the reaction is carried out. The heat collecting unit is connected with a heating unit through a pipeline, wherein the heating unit is arranged on the drying device, and is used for heating the solid salt waste. Due to the fact that the heat released by the reaction in the synthetic reaction still when the reaction is carried out is collected to be used for heating the solid salt waste, organics and water in the solid salt waste is heated to evaporate, salt in the solid salt waste is separated from other components in the solid salt waste, the salt and the other components are respectively used, and effective treatment is carried out on the solid salt waste. Meanwhile, comprehensive utilization is carried out on waste heat produced in production, and cost of solid salt treatment is reduced.

Description

The production system of isocyanuric acid three-glycidyl ester
Technical field
The utility model relates to the isocyanuric acid three-glycidyl ester production field, is 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, high to acid, alkali and other chemical stability, has good especially crosslinking curing performance.Be containing 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 is generally used as shown in Figure 1, being about to epoxy chloropropane (ECH), cyanuric acid (CA) adds according to a certain ratio in reactor and carries out building-up reactions with appropriate catalyzer, obtain intermediate product 1,3,5-tri-(1 '-chloro-2 '-hydroxyl-propyl) chlorinated isocyanurates, again intermediate product and solid sodium hydroxide generation cyclization are obtained to the mixture that contains 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, comprise NaCl, ECH, H 2the Multiple components such as O, especially ECH are poisonous volatile substances, as directly toppled 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): in the document of 56-58, disclosed employing adds the ECH that suction filtration is removed in solid salt refuse after methanol extraction and makes industrial salt (referring to its open file Fig. 1), although the method can effectively be removed the ECH organism in solid salt refuse, but the NaCl rate of recovery is low, Gu because also contain the moisture contained in part moisture and methyl alcohol in the salt refuse, therefore can make part NaCl soluble in water, be difficult to reclaim.In addition, along with the reuse number of times raising of extracting mother liquid, produce the salt rate and also descending.Simultaneously, from industrialization angle Industrial Salt itself, be worth not highly, 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 purpose of this utility model is to provide a kind of production system of isocyanuric acid three-glycidyl ester, and the solid salt refuse produced in producing is processed, 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 filtered for the mixture after reaction in the cyclization still is finished, it is characterized in that: this production system also comprise filtration unit is filtered after remaining solid salt refuse carry out the drying installation of heat treated and liberated heat is collected when reacting in synthesis reaction vessel thermal-arrest unit, this thermal-arrest unit is connected with the heating unit that adds thermosetting salt refuse arranged on drying installation by pipeline.
In the application, by liberated heat when reacting in synthesis reaction vessel, collected for adding thermosetting salt refuse, make organism and moisture in solid salt refuse be subject to thermal evaporation, thereby make the salinity in solid salt refuse be separated with other components, and then utilized respectively, thereby solid salt refuse is effectively processed.The waste heat produced in producing is fully utilized simultaneously, reduced the cost that solid salt is processed.
The accompanying drawing explanation
Fig. 1 is the production technological process that TGIC is traditional;
Fig. 2 is structural representation of the present utility model.
Embodiment
The application's purpose is to provide a kind of production system of isocyanuric acid three-glycidyl ester, says accurately for a kind of and can carry out to the solid salt refuse produced in producing the effectively production system of the isocyanuric acid three-glycidyl ester of processing.So far in TGIC production, solid salt refuse can not get effective processing, its reason mainly contain following some: in first TGIC production process, produce to produce the organic species number and the number change that contain in solid salt refuse larger for each batch, therefore the salt refuse is not a stable mixture formed admittedly, therefore can not directly as product or raw material, be applied; It two is in prior art, also not find to carry out effective Separation and Recovery and each component reclaimed to be carried out to the approach effectively utilized solid salt refuse, therefore mostly adopts to burn or calcining is processed.The scheme adopted in the application, as shown in Figure 2, a kind of production system of isocyanuric acid three-glycidyl ester, comprise the filtration unit 13 filtered for the mixture to after the interior reaction end of cyclization still 12, this production system also comprise filtration unit 13 is filtered after remaining solid salt refuse carry out the drying installation 14 of heat treated and liberated heat is collected when reacting in synthesis reaction vessel 11 thermal-arrest unit 20, this thermal-arrest unit 20 is connected with the heating unit that adds thermosetting salt refuse of setting on drying installation 14 by pipeline.Like this by solid salt refuse being carried out to heat treated drying installation 14 is interior, make the organic phase in solid salt refuse evaporate and separate with moisture, thereby obtain the dry salt that volatile content is extremely low, because dry salt volatile content is extremely low, therefore raw materials for production that can be using it as frostproofer for building or raising agent, and the organism of separating can be again as the raw material of building-up reactions.In the application, by the solid salt refuse in producing, processed recycling, and the waste heat that building-up reactions in producing is produced fully utilized, thereby realized cleaner production and the energy-saving and emission-reduction of TGIC.Difference due to 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 drying installation and processed, in this application, carry out the crystallization filtration treatment by the mixture that interior reaction obtains after finishing to cyclization still 12 in filtration unit 13, obtain solid phase and be the solid waste (wet salt) in the application, filter and make cyclization obtain moisture and the complete crystallization of salinity in mixed system by crystallization, the solid phase that filtration obtains is by 82~83% NaCl, the ECH of 4% left and right, the H of 12% left and right 2o and micro-catalyst combination form, and obtain not containing in liquid phase or containing salt hardly and moisture, make salinity, moisture separate fully with TGIC, byproduct of reaction, just can not produce solid salt refuse in other operation sequences like this.Simultaneously, the utility model adopts the method for physical sepn to be processed solid salt refuse, produces the salt rate and can reach more than 80%, need consider the variation of its component concentration while 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 when this production system also comprises heat treated, escaping gas carries out the organism recovery unit 30 of condensation recovery.Described organism recovery unit 30 comprises the interior escaping gas of drying installation 14 is carried out to 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 and is connected with the second condenser 34 inlet mouths, 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 is delivered to respectively tripping device 36 and carries out the component separation, separates to obtain organic phase and be delivered to that synthesis reaction vessel 11 is interior participates in reaction again as raw material.The gas (that is organism and moisture of volatilization) produced during 30 pairs of heat treated of organism recovery unit by arranging carries out recycling, due to the liquid hot water of more employings when the actually operating as heat-conducting fluid, temperature when solid salt refuse is carried out to heat treated can't be higher like this, therefore, for guaranteeing that the organism in solid salt refuse can be steamed recovery fully, in the application, adopt 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 organism is reclaimed by complete evaporative condenser first, second, during due to heat treated, evaporation escaping gas amount is larger, by most of gas is collected in the interior condensation of the first condenser 31 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 meet 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 consist 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 and is connected by rising pipe 21 and heat storage can 22 for storing heat-conducting fluid, described heating unit is that drying installation 14 perisporiums and/or inner the second cavity for holding heat-conducting fluid arranged combine, described the second cavity is by connecting tube 23, 24 and the pump housing 25 form with heat storage can 22 circulation path that heat-conducting fluids circulate, that is, heat storage can 22 water outlets are connected and are connected with the water inlet of the second cavity on drying installation 14 by connecting tube 23, the water outlet of the second cavity on drying installation 14 is connected and is connected with heat storage can 22 water-ins by connecting tube 24, the pump housing 25 is set on connecting tube 24.First and second cavity here can be by the sandwich structure arranged on synthesis reaction vessel 11 and drying installation 14 perisporiums for holding hot-fluid.Due to required heat when liberated heat is greater than solid salt refuse heat treated of when reaction in synthesis reaction vessel, therefore be provided with heat storage can 22 in the application, heat storage can 22 and heating unit are passed through to connecting tube 23,24 and little water circulation path of the pump housing 25 formation, thereby solid salt refuse is carried out to 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 to 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 in this system, temperature and the vacuum tightness on solid salt refuse heat treated is larger on the impact of producing the salt rate, 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 utility model purpose.
When concrete operations, mixture in cyclization still 12 is placed in filtration unit 13 and carries out the crystallization filtration, the wet salt (consolidating the salt refuse) obtained is placed in rake type drier, be provided with stirring mechanism in rake type drier, dryer cavity is bilayer structure, can lead to hot water in interlayer, combination of lumens becomes the second cavity, start vacuum pump 33 and first, two condensers 31, 34 pairs of rake type driers are vacuumized, as reach-0.08Mpa of vacuum tightness, open the inlet valve arranged on rake type drier, thereby the wet salt in rake type drier is heated, wet salt is heated gradually and heats up, organism and moisture are constantly overflowed and are entered first from evaporation in material, two condensers 31, 34 and main, secondary liquid trap 32, collection is condensed in 35, after heat treated after a while, organic constituent in wet salt and moisture are evaporated complete, obtain industrial dry salt (moisture below 3%), close the inlet valve and the vacuum pump 33 that arrange on rake type drier, take out the raw materials for production that the interior dry salt of rake type drier can be used as frostproofer for building and raising agent.The liquid of collecting in major and minor liquid trap 32,35 is inserted in tripping device 36 and carried out stratification, then the organic phase of separation is again dropped in synthesis reaction vessel 11 and reacted, the water of separation can be used as again water of productive use.
At present, the dry salt obtained by the solid salt refuse of aforesaid operations processing is to detect through Anhui Province's product quality supervision and testing institute, and 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, solid salt refuse, reclaims altogether more than 80 tons of dry salt, the ECH3.6 ton, and accumulative total reduces 85 tons of solid waste discharges, is more than 90,000 yuan of enterprise's additional incomes.
The utility model can effectively be realized solid salt refuse in isocyanuric acid three-glycidyl ester production is processed in a word, the waste heat that solid salt refuse during TGIC is produced and reaction produce carries out recycling, realize cleaner production, production energy-saving and green production, improve the economic benefit that TGIC produces.

Claims (7)

1. the production system of an isocyanuric acid three-glycidyl ester, comprise the filtration unit (13) filtered for the mixture after reaction in cyclization still (12) is finished, it is characterized in that: this production system also comprise filtration unit (13) is filtered after remaining solid salt refuse carry out the drying installation (14) of heat treated and liberated heat is collected when reacting in synthesis reaction vessel (11) thermal-arrest unit (20), this thermal-arrest unit (20) is connected by the upper heating unit that adds thermosetting salt refuse arranged of pipeline and drying installation (14).
2. the production system of isocyanuric acid three-glycidyl ester as claimed in claim 1, it is characterized in that: when this production system also comprises heat treated, escaping gas carries out the organism recovery unit (30) of condensation recovery.
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 and is connected by rising pipe (21) and heat storage can (22) for storing heat-conducting fluid, described heating unit is that drying installation (14) perisporium and/or inner the second cavity for holding heat-conducting fluid arranged combine, described the second cavity is by connecting tube (23, 24) and the pump housing (25) and heat storage can (22) form 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 to 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 and is connected with the second condenser (34) inlet mouth, 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) and carries out the component separation, separates to obtain organic phase and be delivered in 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 6, it is characterized in that: described drying installation (14) is rake type drier.
CN 201220639967 2012-11-28 2012-11-28 Production system of isocyanuric acid tri-glycidyl ester Expired - Fee Related CN202989024U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102964341A (en) * 2012-11-28 2013-03-13 黄山锦峰实业有限公司 Production system of triglycidyl isocyanurate
CN114315809A (en) * 2020-09-29 2022-04-12 湖南云科化工有限公司 Preparation method of triglycidyl isocyanurate

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102964341A (en) * 2012-11-28 2013-03-13 黄山锦峰实业有限公司 Production system of triglycidyl isocyanurate
CN102964341B (en) * 2012-11-28 2016-02-24 黄山锦峰实业有限公司 The production system of isocyanuric acid three-glycidyl ester
CN114315809A (en) * 2020-09-29 2022-04-12 湖南云科化工有限公司 Preparation method of triglycidyl isocyanurate
CN114315809B (en) * 2020-09-29 2023-12-15 湖南云科化工有限公司 Preparation method of triglycidyl isocyanurate

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