CN101781237B - Method for refining J acid by using multi-functional integrated device - Google Patents
Method for refining J acid by using multi-functional integrated device Download PDFInfo
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- CN101781237B CN101781237B CN2009102451334A CN200910245133A CN101781237B CN 101781237 B CN101781237 B CN 101781237B CN 2009102451334 A CN2009102451334 A CN 2009102451334A CN 200910245133 A CN200910245133 A CN 200910245133A CN 101781237 B CN101781237 B CN 101781237B
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- washing
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- 238000000034 method Methods 0.000 title claims abstract description 48
- KYARBIJYVGJZLB-UHFFFAOYSA-N 7-amino-4-hydroxy-2-naphthalenesulfonic acid Chemical compound OC1=CC(S(O)(=O)=O)=CC2=CC(N)=CC=C21 KYARBIJYVGJZLB-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 238000007670 refining Methods 0.000 title claims abstract description 13
- 238000005406 washing Methods 0.000 claims abstract description 50
- 238000001914 filtration Methods 0.000 claims abstract description 38
- 238000001035 drying Methods 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000002253 acid Substances 0.000 claims description 41
- 238000003756 stirring Methods 0.000 claims description 13
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 9
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- 239000002826 coolant Substances 0.000 claims description 6
- 239000012065 filter cake Substances 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 6
- 235000017550 sodium carbonate Nutrition 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims description 3
- 230000001458 anti-acid effect Effects 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 239000003518 caustics Substances 0.000 claims description 3
- 238000005260 corrosion Methods 0.000 claims description 3
- 230000007797 corrosion Effects 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 3
- 238000002386 leaching Methods 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 3
- 239000001117 sulphuric acid Substances 0.000 claims description 3
- 235000011149 sulphuric acid Nutrition 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 4
- 238000004090 dissolution Methods 0.000 abstract 4
- 230000020477 pH reduction Effects 0.000 abstract 2
- 238000005185 salting out Methods 0.000 abstract 2
- 239000002994 raw material Substances 0.000 abstract 1
- 239000012043 crude product Substances 0.000 description 5
- 239000000975 dye Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 2
- PCGISRHGYLRXSR-UHFFFAOYSA-N 4-hydroxy-7-[(5-hydroxy-7-sulfonaphthalen-2-yl)carbamoylamino]naphthalene-2-sulfonic acid Chemical compound OC1=CC(S(O)(=O)=O)=CC2=CC(NC(=O)NC=3C=C4C=C(C=C(C4=CC=3)O)S(O)(=O)=O)=CC=C21 PCGISRHGYLRXSR-UHFFFAOYSA-N 0.000 description 1
- HBZVNWNSRNTWPS-UHFFFAOYSA-N 6-amino-4-hydroxynaphthalene-2-sulfonic acid Chemical compound C1=C(S(O)(=O)=O)C=C(O)C2=CC(N)=CC=C21 HBZVNWNSRNTWPS-UHFFFAOYSA-N 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 238000011437 continuous method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention provides a method for refining J acid by using a multi-functional integrated device, which comprises alkaline water dissolution, salting out, filtering, washing, clear water dissolution integrated process and decoloration, filtering, washing integrated process and the acidification, filtering, washing, and drying integrated process, the alkaline water dissolution, salting out, filtering, washing, and clear water dissolution integrated processes are completed in a first multi-functional device integrating filtering, washing and drying into a whole and decoloration, filtering, washing integrated processes are completed in a second multi-functional device integrating filtering, washing and drying into the whole, and the acidification, filtering, washing, drying integrated processes are completed in a third multi-functional device integrating filtering, washing and drying into the whole. The method has the advantages of a small number of devices, small occupied area, high degree of automation, low loss of raw materials, easy realization of large-scale continuous operation and the like, and can be widely applied in dye production, organic chemical industry and other fields.
Description
Technical field
The present invention relates to a kind of method of refining J acid by using multi-functional integrated device, belong to dyestuff technology, organic chemical industry field.
Background technology
Jie's acid is a kind of dyestuff intermediate, can be used for producing two acid that are situated between, carbonyl-j-acid, phenyl Jie acid, substantive dyestuff and reactive dyestuffs etc.Industry crude product intermediary acid content only is about 90%, wherein also contains water, γ acid and some other insolubles, therefore usually need to make with extra care before use, to remove original impurity in the crude product, obtains elaboration Jie acid.
Jie's acid treating comprises mainly that buck dissolves, saltouts, filters, washing, clear water dissolving, decolouring, filtration, washing, acid out, filtration, washing, drying and other steps, wherein, in the filtration in each step, washing, also to repeat repeatedly, simultaneously also with regulating the processes such as temperature and pH value.Existing process for purification, each step separately carries out, and one ton of elaboration Jie of every production acid approximately consumes 1.7～1.8 tons of crude products Jie acid, therefore has the problems such as number of devices is various, floor space large, artificial intensity is high, production efficiency is low, material loss is many.
Current, in the industries such as medicine, chemical industry, agricultural chemicals, food, be widely used a kind of multifunctional equipment that integrates filtration, washing, drying, this equipment can substitute simultaneously and filter and drying plant (suction filter, pressure filter, double cone dryer, loft drier etc.), in same equipment, finish the processes such as stirring, temperature control, filtration, washing, drying, solid discharging, but this equipment also there is not the report of use in Jie's acid treating technique.
Summary of the invention
The object of the invention is to, for Jie's acid treating Track character, and in conjunction with integrating the advantage of the multifunctional equipment of filtration, washing, drying, for DYE PRODUCTION and part organic chemical industry enterprise provide Jie's acid treating that a kind of number of devices is few, floor space is little, level of automation is high, material loss is few, process is continuous method.
Purpose of the present invention realizes by following approach:
A kind of method of refining J acid by using multi-functional integrated device, comprise that buck dissolves-saltouts-filter-wash-clear water dissolving integrating process, decolouring-filter-washing integrating process and acid out-filtration-washing-dry integrating process, filter at the First collection, washing, in the multifunctional equipment that drying is integrated, finishing buck dissolves-saltouts-and filter-wash-clear water dissolving integrating process, filter at second collection, washing, in the multifunctional equipment that drying is integrated, finish decolouring-filtration-washing integrating process, filter at the 3rd collection, washing, finish acid out-filtration-washing-dry integrating process in the multifunctional equipment that drying is integrated.
The described multifunctional equipment that integrates filtration, washing, drying should have the function of stirring, temperature control, filtration, washing, drying, solid discharging, fluid storage simultaneously, and equipment material has antiacid caustic corrosion performance.
Described buck dissolves-saltouts-filter-wash-and clear water dissolving integrating process comprises: integrates to First in the multifunctional equipment of filtration, washing, drying and adds clear water, yellow soda ash and Jie's acid, be warmed up to 70～85 ℃, stirred 0.8～2 hour; After the acid that is situated between is dissolved fully, add yellow soda ash and regulate between pH value to 6.4～7.5, add again sodium-chlor, stir and saltoutd in 0.8～2 hour; After the acid that is situated between is separated out fully, pass into water coolant in the multifunctional equipment chuck temperature be down to 20～27 ℃, under this temperature, filter, after filtering with 8%～12% sodium chloride aqueous solution washing leaching cake 2～4 times; In equipment, add clear water again, be warmed up to 70～85 ℃, stir and dissolved in 0.5～1 hour.
Described decolouring-filtration-washing integrating process comprises: add gac, diatomite and S-WAT in second multifunctional equipment that integrates filtration, washing, drying, its mass ratio is 16: 4: (0.5～1.5), introducing in second multifunctional equipment with Jie's acid after the clear water dissolving in the First multifunctional equipment, maintain the temperature between 50～75 ℃, stir and decoloured in 0.5～2 hour; Then temperature is down to 37～45 ℃ and filters, pass into again 37～45 ℃ of hot wash filter cakes 2～4 times after the filtration, keep filtrate.
Described acid out-filtration-washing-dry integrating process comprises: the filtrate in second multifunctional equipment is introduced the 3rd integrate in the multifunctional equipment of filtration, washing, drying, temperature adjusting to 50～75 ℃, carry out acid out to the sulfuric acid that wherein adds 18%～22%, regulate between pH value to 3～4.2 to the acid that is situated between and all separate out, pass into water coolant in the multifunctional equipment chuck again temperature is down to 18～25 ℃, then filter, add again the dilute sulphuric acid washing filter cake of pH value between 3～4.2 after the filtration 2～4 times; Then equipment is vacuumized, vacuum degree control is at 5～7KPa, and temperature is controlled at 20～50 ℃ and carries out drying, obtains the refining J acid by using product after the drying.
The present invention compared with prior art exists obvious advantage to be:
(1) number of devices is few, the installation site is compact, floor space is little; (2) each integrating process can be controlled separately, and each integrating process can be together in series to circulate on a large scale and work continuously; (3) level of automation is high, manual operation intensity is little, production efficiency is high; (4) material loss is few.
Description of drawings
Fig. 1 is a kind of schematic flow sheet of refining J acid by using multi-functional integrated device method.
Embodiment
Also describe by reference to the accompanying drawings the present invention in detail below by specific embodiment.
Referring to accompanying drawing 1, Jie's acid treating process is divided into buck dissolves-saltouts-filter-wash-clear water dissolving integrating process, decolouring-filtration-washing integrating process and acid out-filtration-washing-dry integrating process, in three multifunctional equipments that integrate filtration, washing, drying, finish respectively above-mentioned each integrating process, multifunctional equipment should have the function of stirring, temperature control, filtration, washing, drying, solid discharging, fluid storage simultaneously, and equipment material has antiacid caustic corrosion performance.
Integrate to First and add clear water, yellow soda ash and Jie's acid in the multifunctional equipment of filtration, washing, drying, be warmed up to 80 ℃, stirred 1 hour; After the acid that is situated between is dissolved fully, add yellow soda ash and regulate pH value to 6.5, add again sodium-chlor, stir and saltoutd in 1 hour; After the acid that is situated between is separated out fully, pass into water coolant in the multifunctional equipment chuck temperature be down to 23 ℃, under this temperature, filter, after filtering with 10% sodium chloride aqueous solution washing leaching cake 3 times; In equipment, add clear water again, be warmed up to 80 ℃, stir and dissolved in 1 hour.
In second multifunctional equipment that integrates filtration, washing, drying, add gac, diatomite and S-WAT, its mass ratio is 16: 4: 1, introducing in second multifunctional equipment with Jie's acid after the clear water dissolving in the First multifunctional equipment, maintain the temperature at 60 ℃, stir and decoloured in 1 hour; Then temperature is down to 40 ℃ and filters, pass into again 40 ℃ of hot wash filter cakes 2～4 times after the filtration, keep filtrate.
Filtrate in second multifunctional equipment is introduced the 3rd to be integrated in the multifunctional equipment of filtration, washing, drying, temperature is controlled at 60 ℃, carry out acid out to the sulfuric acid that wherein adds 20%, regulate pH value to 3.6, acid is all separated out to being situated between, pass into water coolant in the multifunctional equipment chuck again temperature is down to 22 ℃, then filter, add again pH value after the filtration and be 3.6 dilute sulphuric acid washing filter cake 2 times; Then equipment is vacuumized, vacuum degree control is at 5KPa, and temperature is controlled at 20 ℃ and carries out drying, obtains the refining J acid by using product after the drying.
By implementing method of the present invention, sour chromatogram content is less than 95% in the situation that crude product is situated between, and the be situated between chromatogram content of acid of elaboration has been brought up to more than 99.7%, and produces the acid that is situated between of one ton of elaboration and consume crude product Jie acid and only be 1.15～1.25 tons.
It should be noted that at last: above embodiment is only in order to illustrate the present invention and unrestricted technical scheme described in the invention; Therefore, although this specification sheets has been described in detail the present invention with reference to each above-mentioned embodiment,, those of ordinary skill in the art should be appreciated that still and can make amendment or be equal to replacement the present invention; And all do not break away from technical scheme and the improvement thereof of the spirit and scope of the present invention, and it all should be encompassed in the middle of the claim scope of the present invention.
Claims (4)
1. the method for a refining J acid by using multi-functional integrated device, comprise that buck dissolves-saltouts-filter-wash-clear water dissolving integrating process, decolouring-filter-washing integrating process and acid out-filtration-washing-dry integrating process, it is characterized in that: filter at the First collection, washing, in the multifunctional equipment that drying is integrated, finishing buck dissolves-saltouts-and filter-wash-clear water dissolving integrating process, filter at second collection, washing, in the multifunctional equipment that drying is integrated, finish decolouring-filtration-washing integrating process, filter at the 3rd collection, washing, finish acid out-filtration-washing-dry integrating process in the multifunctional equipment that drying is integrated; The multifunctional equipment that integrates filtration, washing, drying should have the function of stirring, temperature control, filtration, washing, drying, solid discharging, fluid storage simultaneously, and equipment material has antiacid caustic corrosion performance.
2. the method for a kind of refining J acid by using multi-functional integrated device according to claim 1, it is characterized in that: described buck dissolves-saltouts-filter-wash-clear water dissolving integrating process comprises: integrate to First in the multifunctional equipment of filtration, washing, drying and add clear water, yellow soda ash and Jie's acid, be warmed up to 70～85 ℃, stirred 0.8～2 hour; After the acid that is situated between is dissolved fully, add yellow soda ash and regulate between pH value to 6.4～7.5, add again sodium-chlor, stir and saltoutd in 0.8～2 hour; After the acid that is situated between is separated out fully, pass into water coolant in the multifunctional equipment chuck temperature be down to 20～27 ℃, under this temperature, filter, after filtering with 8%～12% sodium chloride aqueous solution washing leaching cake 2～4 times; In equipment, add clear water again, be warmed up to 70～85 ℃, stir and dissolved in 0.5～1 hour.
3. the method for a kind of refining J acid by using multi-functional integrated device according to claim 1, it is characterized in that: described decolouring-filtration-washing integrating process comprises: add gac, diatomite and S-WAT in second multifunctional equipment that integrates filtration, washing, drying, its mass ratio is 16: 4: (0.5～1.5), introducing in second multifunctional equipment with Jie's acid after the clear water dissolving in the First multifunctional equipment, maintain the temperature between 50～75 ℃, stir and decoloured in 0.5～2 hour; Then temperature is down to 37～45 ℃ and filters, pass into again 37～45 ℃ of hot wash filter cakes 2～4 times after the filtration, keep filtrate.
4. the method for a kind of refining J acid by using multi-functional integrated device according to claim 1, it is characterized in that: described acid out-filtration-washing-dry integrating process comprises: the filtrate in second multifunctional equipment is introduced the 3rd collection filter, washing, in the multifunctional equipment that drying is integrated, temperature adjusting to 50～75 ℃, carry out acid out to the sulfuric acid that wherein adds 18%～22%, regulate between pH value to 3～4.2 to the acid that is situated between and all separate out, pass into water coolant in the multifunctional equipment chuck again temperature is down to 18～25 ℃, then filter, add again the dilute sulphuric acid washing filter cake of pH value between 3～4.2 after the filtration 2～4 times; Then equipment is vacuumized, vacuum degree control is at 5～7KPa, and temperature is controlled at 20～50 ℃ and carries out drying, obtains the refining J acid by using product after the drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102451334A CN101781237B (en) | 2009-12-28 | 2009-12-28 | Method for refining J acid by using multi-functional integrated device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102451334A CN101781237B (en) | 2009-12-28 | 2009-12-28 | Method for refining J acid by using multi-functional integrated device |
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| Publication Number | Publication Date |
|---|---|
| CN101781237A CN101781237A (en) | 2010-07-21 |
| CN101781237B true CN101781237B (en) | 2013-04-10 |
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| CN2009102451334A Expired - Fee Related CN101781237B (en) | 2009-12-28 | 2009-12-28 | Method for refining J acid by using multi-functional integrated device |
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| CN101781237A (en) | 2010-07-21 |
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