CN103274971A - Purification method of 5-sulfosalicylic acid - Google Patents
Purification method of 5-sulfosalicylic acid Download PDFInfo
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- CN103274971A CN103274971A CN2013102424013A CN201310242401A CN103274971A CN 103274971 A CN103274971 A CN 103274971A CN 2013102424013 A CN2013102424013 A CN 2013102424013A CN 201310242401 A CN201310242401 A CN 201310242401A CN 103274971 A CN103274971 A CN 103274971A
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- sulphosalicylic acid
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- sulfosalicylic acid
- sulphosalicylic
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Abstract
The invention discloses a purification method of a 5-sulfosalicylic acid. The purification method comprises the following steps: taking industrial-grade 5-sulfosalicylic acid as a raw material, adding a composite cleaning agent made by the company into the raw material, heating, stirring and refluxing, pumping water out and centrifuging after cooling to obtain crude 5-sulfosalicylic acid products, and then obtaining purified 5-sulfosalicylic acid through collecting 5-sulfosalicylic acid products in a conventional method, wherein the purity of the 5-sulfosalicylic acid obtained by the purification method is larger than 99.5%. Compared with the prior art, the purification method has a safe and convenient purification process, saves energy and reduces emission; the composite cleaning agent can be recycled after being activated, so that the requirements of green chemical industry and environment protection are met; and the purified 5-sulfosalicylic acid product is stable in quality, and has an industrial production prospect.
Description
Technical field
The present invention relates to a kind of purification process of 5-sulphosalicylic acid.
Background technology
The 5-sulphosalicylic acid is called for short sulphosalicylic acid, claims 2-hydroxy-5-sulfobenzoic acid again, and English 5-sulphosalicylic acid by name is mainly used in the dyestuff manufacturing, tensio-active agent, catalyzer, medicine intermediate etc.The 5-sulphosalicylic acid is in dyestuffs industries, for the manufacture of the intermediate of tensio-active agent; In medicine intermediate, be doxycycline, the raw material of several formulations such as methacycline; The 5-sulphosalicylic acid still is the developer of a metal ion species, can be used for measuring manganese, multiple metal ion such as lead.
Its structural formula of 5-sulphosalicylic acid is as follows:
In the prior art, the report of 5-sulphosalicylic acid method of wastewater treatment is more, but discloses very few to the research of its method of purification.Because the solubleness of 5-sulphosalicylic acid in water, ethanol, ether is all very big, and numerous metal ions are had very high sensitivity, technical grade product has more foreign ion usually again, has increased the purification difficulty of 5-sulphosalicylic acid." introduced the method that the saturated NaCl solution washing of a kind of usefulness 5-sulphosalicylic acid is purified in the modern chemistry reagent handbook, but the product that obtains with this method purification can't reach industry standard HG3-991-84, does not have the prospect of industrialization; Chinese patent 96101640.X discloses a kind of directly the purification by industrial goods and has produced the method for SILVER REAGENT 5-sulphosalicylic acid and sodium salt thereof, and this method is with industrial goods water heating for dissolving, subcooling crystallization, through centrifugation, filter, concentrate, cooling, crystallization is again by centrifugation, crystallization, drying, purifying obtains SILVER REAGENT 5-sulphosalicylic acid, the product purity height that this method obtains, but complex steps, the time is long, energy consumption is big, the cost height, and the value of suitability for industrialized production is little.
Summary of the invention
Technical problem to be solved by this invention provides a kind of purification process of 5-sulphosalicylic acid, and is low to overcome in the prior art 5-sulphosalicylic acid purified product purity, complex operation, and energy consumption is big, the deficiency that cost is high.
Technical conceive of the present invention is such:
The present invention is raw material with technical grade 5-sulphosalicylic acid, and the composite purifying agent heated and stirred that adds our company's independent research refluxes, and through draining the centrifugal 5-sulphosalicylic acid crude product that gets, adopts ordinary method to collect the 5-sulphosalicylic acid that obtains purifying then after cooling.
Technical scheme of the present invention: a kind of purification process of 5-sulphosalicylic acid, comprise the steps: composite purifying agent is added in the technical grade 5-sulphosalicylic acid, be heated to 60～70 ℃ of stirring and refluxing 4～6h, drain the centrifugal 5-sulphosalicylic acid crude product that gets after being cooled to room temperature, saturated aqueous solution is made in dissolving in this 5-sulphosalicylic acid crude product adding deionized water, add gac again and stir 3～4h, remove by filter gac, get filtrate in 65～70 ℃ of concentrating under reduced pressure, obtain the 5-sulphosalicylic acid of purifying;
Wherein: described composite purifying agent is the mixture of N,N-DIMETHYLACETAMIDE, isoamyl acetate, ethyl acetate, butylacetate, hexone and dimethyl phthalate, the mol ratio of its mixing is: 0.3～0.4:0,2～0.3:1:0.6～0.7:0,2～0.3:0.4～0.5, optimum ratio are 0.365:0.279:1:0.672:0.255:0.436.
According to the present invention, the mass volume ratio of described 5-sulphosalicylic acid and composite purifying agent is 1:0.35-0.45, g/mL.The mass volume ratio of described 5-sulphosalicylic acid and deionized water is 1:0.5-0.7, g/mL.The mass ratio of described 5-sulphosalicylic acid and gac is 1:0.01-0.02, g/g.
Described gac passes through pre-treatment before use, and this pretreatment process is: 1. by proportioning 5-sulphosalicylic acid: ethyl acetate=0.03～0.05:1, g/mL obtain solution; 2. adopt the solution soaking gac 12～24h of above-mentioned preparation, use twice gac of deionized water drip washing after draining again, to remove muriate, vitriol and the metal ion in the gac, dry for standby then.
The 5-sulphosalicylic acid that purifying of the present invention is used, raw material N,N-DIMETHYLACETAMIDE, isoamyl acetate, ethyl acetate, butylacetate, hexone, dimethyl phthalate and the gac of composite purifying agent all has sale on market, raw material is easy to get, employed composite purifying agent can activate after treatment, can reuse, adopt the 5-sulphosalicylic acid purity of purification process acquisition of the present invention greater than 99.5%.
Beneficial effect of the present invention:
1. the composite purifying agent of the independent research of the present invention's employing can effectively be removed 5-sulphosalicylic acid impurities in raw materials, and the 5-sulphosalicylic acid purity of acquisition is greater than 99.5%, and purge process is safe and simple, energy-saving and emission-reduction;
2. activated can the recycling of composite purifying agent of the used independent research of the present invention meets green chemical industry, the protection environment requirement;
3. the 5-sulphosalicylic acid that obtains of purification process of the present invention, constant product quality has industrial production foreground.
Embodiment
The invention will be further described below by embodiment, but embodiment does not limit protection scope of the present invention.
Embodiment 1
The 350ml composite purifying agent is joined in the 1000g technical grade 5-sulphosalicylic acid, be heated to 60 ℃ of stirring and refluxing 4h, be cooled to room temperature by draining the centrifugal 963g5-sulphosalicylic acid crude product that gets, saturated aqueous solution is made in dissolving in this 5-sulphosalicylic acid crude product adding 500mL deionized water, add the 10g activated carbon again and stir 3h, remove by filter activated carbon, get filtrate in 70 ℃ of concentrating under reduced pressure, obtain the white crystals shape product 5-sulphosalicylic acid 929g of purifying, purity 99.53%;
The used composite purifying agent of present embodiment is the mixture of N,N-DIMETHYLACETAMIDE, isoamyl acetate, ethyl acetate, butylacetate, hexone and dimethyl phthalate, and the mol ratio of its mixing is: 0.4:0.3:1:0.7:0.3:0.5.
Embodiment 2
The 400ml composite purifying agent is joined in the 1000g technical grade 5-sulphosalicylic acid, be heated to 65 ℃ of stirring and refluxing 5h, be cooled to room temperature by draining the centrifugal 956g5-sulphosalicylic acid crude product that gets, saturated aqueous solution is made in dissolving in this 5-sulphosalicylic acid crude product adding 600mL deionized water, add the 15g activated carbon again and stir 3.5h, remove by filter activated carbon, get filtrate in 68 ℃ of concentrating under reduced pressure, obtain the white crystals shape product 5-sulphosalicylic acid 917g of purifying, purity 99.59%.
The used composite purifying agent of present embodiment is the mixture of N,N-DIMETHYLACETAMIDE, isoamyl acetate, ethyl acetate, butylacetate, hexone and dimethyl phthalate, and the mol ratio of its mixing is: 0.3:0.2:1:0.6:0.2:0.4.
Embodiment 3
The 450ml composite purifying agent is joined in the 1000g technical grade 5-sulphosalicylic acid, be heated to 70 ℃ of stirring and refluxing 6h, be cooled to room temperature by draining the centrifugal 945g5-sulphosalicylic acid crude product that gets, saturated aqueous solution is made in dissolving in this 5-sulphosalicylic acid crude product adding 700mL deionized water, add the 20g activated carbon again and stir 4h, remove by filter activated carbon, get filtrate in 65 ℃ of concentrating under reduced pressure, obtain the white crystals shape product 5-sulphosalicylic acid 903g of purifying, purity 99.62%.
The used composite purifying agent of present embodiment is the mixture of N,N-DIMETHYLACETAMIDE, isoamyl acetate, ethyl acetate, butylacetate, hexone and dimethyl phthalate, and the mol ratio of its mixing is: 0.35:0.25:1:0.65:0.25:0.45.
Embodiment 4
The 450ml composite purifying agent is joined in the 1000g technical grade 5-sulphosalicylic acid, be heated to 70 ℃ of stirring and refluxing 6h, be cooled to room temperature by draining the centrifugal 945g5-sulphosalicylic acid crude product that gets, saturated aqueous solution is made in dissolving in this 5-sulphosalicylic acid crude product adding 700mL deionized water, add the 20g activated carbon again and stir 4h, remove by filter activated carbon, get filtrate in 65 ℃ of concentrating under reduced pressure, obtain the white crystals shape product 5-sulphosalicylic acid 900g of purifying, purity 99.90%.
The used composite purifying agent of present embodiment is the mixture of N,N-DIMETHYLACETAMIDE, isoamyl acetate, ethyl acetate, butylacetate, hexone and dimethyl phthalate, and the mol ratio of its mixing is: 0.365:0.279:1:0.672:0.255:0.436.
Need to prove that above embodiment is only unrestricted in order to technical scheme of the present invention to be described.Although with reference to preferred embodiment the present invention is had been described in detail, those of ordinary skill in the art is to be understood that, can make amendment or be equal to replacement the technical scheme of invention, and not break away from the scope of technical solution of the present invention, it all should be encompassed in the claim scope of the present invention.
Claims (5)
1. the purification process of a 5-sulphosalicylic acid, it is characterized in that, comprise the steps: composite purifying agent is added in the technical grade 5-sulphosalicylic acid, be heated to 60～70 ℃ of stirring and refluxing 4～6h, be cooled to and drain centrifugal 5-sulphosalicylic acid crude product after the room temperature, this 5-sulphosalicylic acid crude product is added in deionized water dissolving make saturated aqueous solution, add gac again and stir 3～4h, remove by filter gac, get filtrate in 65～70 ℃ of concentrating under reduced pressure, obtain the 5-sulphosalicylic acid of purifying;
Wherein: described composite purifying agent is the mixture of N,N-DIMETHYLACETAMIDE, isoamyl acetate, ethyl acetate, butylacetate, hexone and dimethyl phthalate, and the mol ratio of its mixing is: 0.3～0.4:0.2～0.3:1:0.6～0.7:0.2～0.3:0.4～0.5.
2. method according to claim 1 is characterized in that, the mass volume ratio of described 5-sulphosalicylic acid and composite purifying agent is 1:0.35-0.45, g/mL.
3. method according to claim 1 is characterized in that, the mass volume ratio of described 5-sulphosalicylic acid and deionized water is 1:0.5-0.7, g/mL.
4. method according to claim 1 is characterized in that, the mass ratio of described 5-sulphosalicylic acid and gac is 1:0.01-0.02, g/g.
5. method according to claim 1 is characterized in that, described gac passes through pre-treatment before use, and this pretreatment process is:
1. by proportioning 5-sulphosalicylic acid: ethyl acetate=0.03～0.05:1, g/mL obtain solution;
2. adopt the solution soaking gac 12～24h of above-mentioned preparation, use twice gac of deionized water drip washing after draining again, then dry for standby.
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| CN201310242401.3A CN103274971B (en) | 2013-06-19 | 2013-06-19 | Purification method of 5-sulfosalicylic acid |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105348154A (en) * | 2014-12-10 | 2016-02-24 | 开封制药(集团)有限公司 | Method for recycling sulfosalicylic acid from doxycycline production waste liquid |
| CN108822003A (en) * | 2018-05-31 | 2018-11-16 | 成都市科隆化学品有限公司 | A kind of purifying technique of sulfosalicylic acid |
| CN108863856A (en) * | 2018-06-15 | 2018-11-23 | 永华化学科技（江苏）有限公司 | A kind of analytical reagents 5-sulphosalicylic acid method of purification |
| CN110372548A (en) * | 2018-04-12 | 2019-10-25 | 南京化学试剂股份有限公司 | A kind of refining methd of 5-sulphosalicylic acid |
Citations (2)
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| CN1137517A (en) * | 1996-01-27 | 1996-12-11 | 河南省科学院化学研究所 | Preparing reagent grade sulfosalicylic acid and its sodium salt by industrial product epuration |
| US5596128A (en) * | 1990-10-12 | 1997-01-21 | Konishi Chemical Ind. Co., Ltd. | Sulfonating agent and sulfonation process |
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2013
- 2013-06-19 CN CN201310242401.3A patent/CN103274971B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5596128A (en) * | 1990-10-12 | 1997-01-21 | Konishi Chemical Ind. Co., Ltd. | Sulfonating agent and sulfonation process |
| CN1137517A (en) * | 1996-01-27 | 1996-12-11 | 河南省科学院化学研究所 | Preparing reagent grade sulfosalicylic acid and its sodium salt by industrial product epuration |
Non-Patent Citations (1)
| Title |
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| 邢东志: "5-磺基水杨酸合成工艺的改进", 《开封医专学报》, vol. 15, no. 1, 31 December 1996 (1996-12-31), pages 23 - 24 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105348154A (en) * | 2014-12-10 | 2016-02-24 | 开封制药(集团)有限公司 | Method for recycling sulfosalicylic acid from doxycycline production waste liquid |
| CN110372548A (en) * | 2018-04-12 | 2019-10-25 | 南京化学试剂股份有限公司 | A kind of refining methd of 5-sulphosalicylic acid |
| CN108822003A (en) * | 2018-05-31 | 2018-11-16 | 成都市科隆化学品有限公司 | A kind of purifying technique of sulfosalicylic acid |
| CN108863856A (en) * | 2018-06-15 | 2018-11-23 | 永华化学科技（江苏）有限公司 | A kind of analytical reagents 5-sulphosalicylic acid method of purification |
| CN108863856B (en) * | 2018-06-15 | 2021-06-01 | 永华化学股份有限公司 | Purification method of analytically pure reagent 5-sulfosalicylic acid |
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