CN212246238U - By-product ammonium sulfate refining plant in isophthalonitrile production - Google Patents
By-product ammonium sulfate refining plant in isophthalonitrile production Download PDFInfo
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- CN212246238U CN212246238U CN202020254887.8U CN202020254887U CN212246238U CN 212246238 U CN212246238 U CN 212246238U CN 202020254887 U CN202020254887 U CN 202020254887U CN 212246238 U CN212246238 U CN 212246238U
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Abstract
The utility model belongs to the technical field of fine chemistry industry and pesticide, concretely relates to by-product ammonium sulfate refining plant in isophthalonitrile production, including the crude ammonium sulfate that connects gradually dissolve cauldron, the refined cauldron of ammonium sulfate, plate frame filter and ammonium sulfate evaporation crystallization cauldron, be equipped with crude ammonium sulfate ammonia dog-house and water inlet on the crude ammonium sulfate dissolves the cauldron, be equipped with the diatomaceous earth dog-house on the refined cauldron of ammonium sulfate, the refined cauldron top of ammonium sulfate is connected with hydrogen peroxide solution storage tank, aqueous ammonia storage tank and dilute sulfuric acid storage tank respectively, ammonium sulfate evaporation crystallization cauldron top and vacuum system are connected, and ammonium sulfate evaporation crystallization cauldron bottom is connected with high-speed centrifuge. The utility model discloses simple easy operation, work efficiency is high, can effectively retrieve boil-off gas, avoids the pollution to the environment, but the content greatly reduced of the total cyanide of ammonium sulfate salt after the processing, and colour whiteness shows the improvement, and the well complex cyanogen concentration greatly reduced of the ammonium sulfate salt after the refining can alleviate ambient pressure.
Description
Technical Field
The utility model belongs to the technical field of fine chemistry industry and pesticide, concretely relates to by-product ammonium sulfate refining plant in isophthalonitrile production.
Background
The molecular formula of the isophthalonitrile is C8H4N2The material is white needle crystal. Slightly soluble in hot water, soluble in hot ethanol, diethyl ether, benzene and chloroform. The product is used as raw material for preparing pesticide chlorothalonil and antiseptic, and also as curing agent for polyurethane resin and epoxy resin. The mixed gas composed of m-xylene, ammonia and air is passed through a vanadium-based catalyst, the reaction temperature is 400-425 ℃, and the contact time is about 3 s. The m-phthalonitrile with the purity of more than 91 percent is obtained, and the yield is more than 93 percent. The method is also the most main production method of the prior m-phthalonitrile, and in order to improve the conversion rate of m-xylene in the reaction process, the reaction molar ratio of the m-xylene, ammonia gas and air is 1:5.5: 35. This causes an excess of ammonia gas, and it is currently common practice to use dilute sulfuric acid to absorb the excess ammonia gas to produce ammonium sulfate. The reaction equation for the preparation of isophthalonitrile is as follows:
due to the excessive ammonia and air, a small amount of m-phthalonitrile is excessively oxidized to generate free-CN and short-chain organic matters, so that COD (chemical oxygen demand) and total cyanogen in the recovered ammonium sulfate are high, and if the ammonium sulfate is directly sold as a byproduct, the product quality is not high and the value is low; meanwhile, if the complex cyanogen is not used properly, the complex cyanogen enters the environment and generates potential danger to soil and water sources.
SUMMERY OF THE UTILITY MODEL
The to-be-solved technical problem of the utility model is: overcome prior art's not enough, provide a by-product ammonium sulfate refining plant in isophthalonitrile production, can solve COD and the higher problem of total complex cyanogen in the ammonium sulfate of retrieving, improve ammonium sulfate product quality, alleviate environmental pressure.
The utility model discloses an adopt following technical scheme to realize:
m-phthalonitrile production in byproduct ammonium sulfate refining plant, including the crude ammonium sulfate that connects gradually dissolve cauldron, the refined cauldron of ammonium sulfate, plate filter and ammonium sulfate evaporation crystallization cauldron, be equipped with crude ammonium sulfate ammonia dog-house and water inlet on the crude ammonium sulfate dissolves the cauldron, be equipped with the diatomaceous earth dog-house on the refined cauldron of ammonium sulfate, the refined cauldron top of ammonium sulfate is connected with hydrogen peroxide solution storage tank, aqueous ammonia storage tank and dilute sulfuric acid storage tank respectively, ammonium sulfate evaporation crystallization cauldron top and vacuum system are connected, ammonium sulfate evaporation crystallization cauldron bottom is connected with high speed centrifuge.
Preferably, a crude ammonium sulfate delivery pump is arranged between the crude ammonium sulfate dissolving kettle and the ammonium sulfate refining kettle; an ammonium sulfate delivery pump is arranged between the ammonium sulfate refining kettle and the plate frame filter.
Preferably, the top of the ammonium sulfate evaporative crystallization kettle is sequentially connected with a first-stage condenser and a second-stage condenser, and the second-stage condenser is connected with a vacuum system. The first-stage condenser and the second-stage condenser are both connected with the condensed water collecting tank.
During operation, adding crude ammonium sulfate and water into a crude ammonium sulfate dissolving kettle, dissolving the crude ammonium sulfate into a 20-40% aqueous solution, stirring for full dissolution, pumping the dissolved crude ammonium sulfate solution into an ammonium sulfate refining kettle through a crude ammonium sulfate delivery pump, dropwise adding dilute sulfuric acid to adjust the pH to 3-5, adding hydrogen peroxide, heating to 30-50 ℃ for thermal insulation oxidation for 3-5h, adding ammonia water to adjust the pH to 6-7 after oxidation, adding diatomite from a diatomite feeding port, stirring for 0.5-1h under thermal insulation, delivering the ammonium sulfate solution completely oxidized and decomposed to a plate frame filter by an ammonium sulfate delivery pump for plate frame filter pressing, separating flocculate, pumping the filtered ammonium sulfate solution into an ammonium sulfate evaporation crystallization kettle, heating to 70-80 ℃, adjusting the vacuum degree to-0.08-0.09 MPa by a vacuum system, and (3) carrying out reduced pressure evaporation, condensing the gas from the top of the ammonium sulfate evaporation crystallization kettle through a primary condenser and a secondary condenser, then recovering the gas to a condensate water collecting tank, introducing cooling circulating water into a jacket of the ammonium sulfate evaporation crystallization kettle after evaporation is finished, stirring and cooling the gas to normal temperature, and centrifuging an ammonium sulfate solution containing crystals by a high-speed centrifuge to obtain fine ammonium sulfate.
Compared with the prior art, the beneficial effects of the utility model are as follows:
1. the utility model discloses can handle organic complex and the cyanide of colour development in the ammonium sulfate salt, but the content greatly reduced of the total cyanide of ammonium sulfate salt after the processing, colour whiteness is showing and is improving, and the well complex cyanogen and the COD concentration greatly reduced of the ammonium sulfate salt after the refining can alleviate the ambient pressure.
2. The utility model has the advantages of being scientific and reasonable in structure, simple easy operation, work efficiency is high, can effectively retrieve the boil-off gas, avoids the pollution to the environment.
Drawings
Fig. 1 is a schematic structural view of the present invention;
in the figure: 1. a crude product ammonium sulfate dissolving kettle; 101. a crude ammonium sulfate ammonia feeding port; 102. a water inlet; 2. a crude ammonium sulfate delivery pump; 3. a hydrogen peroxide storage tank; 4. an ammonia water storage tank; 5. a dilute sulfuric acid storage tank; 6. an ammonium sulfate refining kettle; 601. a diatomite feeding port; 7. an ammonium sulfate delivery pump; 8. a plate frame filter; 9. evaporating and crystallizing the ammonium sulfate in a kettle; 10. a first-stage condenser; 11. a secondary condenser; 12. a vacuum system; 13. a condensed water collection tank; 14. a high-speed centrifuge.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and examples.
As shown in fig. 1, m-phthalonitrile production in byproduct ammonium sulfate refining plant, including the crude ammonium sulfate solution cauldron 1 that connects gradually, the refined cauldron 6 of ammonium sulfate, plate and frame filter 8 and ammonium sulfate evaporation crystallization cauldron 9, be equipped with crude ammonium sulfate ammonia dog-house 101 and water entry 102 on the crude ammonium sulfate solution cauldron 1, be equipped with diatomaceous earth dog-house 601 on the refined cauldron 6 of ammonium sulfate, 6 tops of the refined cauldron of ammonium sulfate are connected with hydrogen peroxide solution storage tank 3, aqueous ammonia storage tank 4 and dilute sulphuric acid storage tank 5 respectively, ammonium sulfate evaporation crystallization cauldron 9 tops be connected with one-level condenser 10 and secondary condenser 11 in proper order, secondary condenser 11 is connected with vacuum system 12, one-level condenser 10 and secondary condenser 11 all be connected with condensate collection tank 13, ammonium sulfate evaporation crystallization cauldron 9 bottoms are connected with high speed centrifuge 14.
A crude ammonium sulfate delivery pump 2 is arranged between the crude ammonium sulfate dissolving kettle 1 and the ammonium sulfate refining kettle 6; an ammonium sulfate delivery pump 7 is arranged between the ammonium sulfate refining kettle 6 and the plate frame filter 8.
During operation, crude ammonium sulfate and water are added into a crude ammonium sulfate dissolving kettle 1, the crude ammonium sulfate is dissolved into a 20-40% aqueous solution, the solution is fully dissolved by stirring, the dissolved crude ammonium sulfate solution is pumped into an ammonium sulfate refining kettle 6 through a crude ammonium sulfate delivery pump 2, dilute sulfuric acid is dripped to adjust the pH value to 3-5, hydrogen peroxide is added, the solution is heated to 30-50 ℃ for heat preservation and oxidation for 3-5h, ammonia water is added after the oxidation is finished to adjust the pH value to 6-7, then diatomite is added from a diatomite feeding port 601, the solution is stirred for 0.5-1h by heat preservation, the ammonium sulfate solution which is completely oxidized and decomposed is delivered to a plate frame filter 8 by an ammonium sulfate delivery pump 7 for plate frame filter pressing, flocculate is separated, the filtered ammonium sulfate solution is pumped into an ammonium sulfate evaporation crystallization kettle 9, the solution is heated to 70-80 ℃, the vacuum degree is adjusted to-0.08, and (3) carrying out reduced pressure evaporation, condensing the gas from the top of the ammonium sulfate evaporative crystallization kettle 9 through a primary condenser 10 and a secondary condenser 11, then recovering the gas to a condensate water collecting tank 13, introducing cooling circulating water into a jacket of the ammonium sulfate evaporative crystallization kettle 9 after evaporation is finished, stirring and cooling the gas to normal temperature, and centrifuging an ammonium sulfate solution containing crystals by a high-speed centrifuge 14 to obtain fine ammonium sulfate.
Of course, the above description is only a preferred embodiment of the present invention, and should not be taken as limiting the scope of the embodiments of the present invention. The present invention is not limited to the above examples, and the technical field of the present invention is equivalent to the changes and improvements made in the actual range of the present invention, which should be attributed to the patent coverage of the present invention.
Claims (4)
1. The utility model provides a by-product ammonium sulfate refining plant in isophthalonitrile production which characterized in that: including the crude ammonium sulfate dissolving kettle (1), the refined cauldron of ammonium sulfate (6), plate and frame filter (8) and the ammonium sulfate evaporation crystallization cauldron (9) that connect gradually, be equipped with crude ammonium sulfate ammonia dog-house (101) and water entry (102) on crude ammonium sulfate dissolving kettle (1), be equipped with diatomaceous earth dog-house (601) on the refined cauldron of ammonium sulfate (6), the refined cauldron of ammonium sulfate (6) top is connected with hydrogen peroxide solution storage tank (3), aqueous ammonia storage tank (4) and dilute sulfuric acid storage tank (5) respectively, ammonium sulfate evaporation crystallization cauldron (9) top is connected with vacuum system (12), and ammonium sulfate evaporation crystallization cauldron (9) bottom is connected with high-speed centrifuge (14).
2. The apparatus for refining ammonium sulfate as a byproduct in the production of isophthalonitrile according to claim 1, wherein: a crude ammonium sulfate delivery pump (2) is arranged between the crude ammonium sulfate dissolving kettle (1) and the ammonium sulfate refining kettle (6); an ammonium sulfate delivery pump (7) is arranged between the ammonium sulfate refining kettle (6) and the plate frame filter (8).
3. The apparatus for refining ammonium sulfate as a byproduct in the production of isophthalonitrile according to claim 1, wherein: the top of the ammonium sulfate evaporation crystallization kettle (9) is sequentially connected with a first-stage condenser (10) and a second-stage condenser (11), and the second-stage condenser (11) is connected with a vacuum system (12).
4. The apparatus for refining ammonium sulfate as a byproduct in the production of isophthalonitrile according to claim 3, wherein: the primary condenser (10) and the secondary condenser (11) are both connected with a condensed water collecting tank (13).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020254887.8U CN212246238U (en) | 2020-03-04 | 2020-03-04 | By-product ammonium sulfate refining plant in isophthalonitrile production |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020254887.8U CN212246238U (en) | 2020-03-04 | 2020-03-04 | By-product ammonium sulfate refining plant in isophthalonitrile production |
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| Publication Number | Publication Date |
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| CN212246238U true CN212246238U (en) | 2020-12-29 |
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| CN202020254887.8U Active CN212246238U (en) | 2020-03-04 | 2020-03-04 | By-product ammonium sulfate refining plant in isophthalonitrile production |
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| CN (1) | CN212246238U (en) |
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- 2020-03-04 CN CN202020254887.8U patent/CN212246238U/en active Active
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