CN110372548A - A kind of refining methd of 5-sulphosalicylic acid - Google Patents
A kind of refining methd of 5-sulphosalicylic acid Download PDFInfo
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- CN110372548A CN110372548A CN201810325931.7A CN201810325931A CN110372548A CN 110372548 A CN110372548 A CN 110372548A CN 201810325931 A CN201810325931 A CN 201810325931A CN 110372548 A CN110372548 A CN 110372548A
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- Prior art keywords
- sulphosalicylic acid
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- ethyl acetate
- deionized water
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/42—Separation; Purification; Stabilisation; Use of additives
- C07C303/44—Separation; Purification
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A kind of refining methd of 5-sulphosalicylic acid is impregnated method includes the following steps: taking 5-sulphosalicylic acid industrial goods with ethyl acetate, centrifuge dripping, ethyl acetate is added in resulting immersion material, centrifuge dripping dries in material and deionized water is added, dissolve drying material sufficiently, active carbon, stirring, filtering is added, obtained concentrate places room temperature, crystallisation by cooling, centrifugal dehydration, drying are to get 5-sulphosalicylic acid sterling.
Description
Technical field
The present invention relates to a kind of techniques that organic acid reagent is prepared by industrial organic acid, the especially essence of 5-sulphosalicylic acid
Method processed.
Background technique
The molecular formula of 5-sulphosalicylic acid is C7H6O6S·2H2O, white crystals or crystalline powder have hygroscopicity, fusing point
120 DEG C, soluble easily in water and ethyl alcohol is dissolved in ether.Iron is met into pink, pyrolytic is at sulfuric acid and salicylic acid.It is widely used in
The fields such as surfactant-intermediate, medicine intermediate, organic catalyst, grease additive.Made in chemical reagent field
For biochemical reagents, analytical reagent and complexing agent etc..Measure aluminium, beryllium, calcium, chromium, copper, iron, lead, magnesium, sodium, titanium, thallium and nitrate.Point
Analyse rare earth metal cerium.Measure the iron contents such as steel raw material iron ore, coal tar, lime stone, clinker.
Since 5-sulphosalicylic acid industrial goods contain a large amount of impurities, color is deeper, when detecting certain ions as reagent, sternly
Ghost image rings the sensitivity of detection, therefore needs to refine industrial goods, to obtain grade product.But 5-sulphosalicylic acid
Solubility in water is very big, acid stronger, has good adsorptivity to metal ion, exists centainly so refining to it
It is difficult.Patent CN1137517A discloses a kind of method for producing SILVER REAGENT sulfosalicylic acid and its sodium salt by industrial goods purification,
By industrial goods sulfosalicylic acid deionized water dissolving, the crystallisation by cooling at 0-10 DEG C is centrifugated through copper centrifuge, will be divided
The crystal separated out be dissolved in be added in deionized water impregnated through sulfuric acid, hydrochloric acid elution, deionized water be washed till neutral active carbon in
It in solution, then filters this solution filtrate and is concentrated, cools down, crystallizes at 60-100 DEG C, by the centrifuge separation of copper centrifuge, knot
Crystalline substance is drying to obtain finished product.This method needs recrystallizing technology twice, and the purity of obtained finished product is only 99.19%, operation stream
Journey is complicated, and product quality is not high.Method disclosed in patent CN103274971A is that technical grade 5- sulfo group is added in composite purifying agent
In salicylic acid, it is heated to reflux 4-6h, is drained after being cooled to room temperature and is centrifuged to obtain 5-sulphosalicylic acid crude product, by the 5-sulphosalicylic acid
Crude product is added dissolution in deionized water and saturated aqueous solution is made, and adds active carbon stirring 3-4h, is filtered to remove active carbon, takes filter
Liquid is concentrated under reduced pressure in 65-70 DEG C, obtains the 5-sulphosalicylic acid of purifying；Wherein: the composite purifying agent is N, N- dimethyl
Acetamide, isoamyl acetate, ethyl acetate, butyl acetate, hexone and repefral mixture,
Its molar ratio mixed are as follows: 0.3-0.4:0.2-0.3:1:0.6-0.7:0.2-0.3:0.4-0.5.This technical operation flow compared with
Long, composite purifying agent subsequent processing is also more troublesome.
Summary of the invention
In order to overcome operating process of the existing technology long, the composite purifying agent subsequent processing of addition is complicated, and product is pure
The problems such as not high is spent, the present invention provides a kind of refining methd of 5-sulphosalicylic acid, specific steps include:
(1) it impregnates, is de- dry: taking 5-sulphosalicylic acid industrial goods, impregnated with ethyl acetate, centrifuge dripping obtains immersion material；
(2) material is washed, takes off and does: ethyl acetate is added into the resulting immersion material of step (1), centrifuge dripping obtains drying object
Material；
(3) it dissolves, filter: deionized water is added into the resulting drying material of step (2), keep drying material sufficiently molten
Solution, obtains lysate, then active carbon is added into gained lysate, and stirring, filtering obtain filter material；
(4) it is concentrated, crystallizes: the resulting filter material of step (3) is concentrated, obtained concentrate places room temperature, cooling knot
Crystalline substance obtains crystallized stock；
(5) it is dehydrated, is dry: the resulting crystallized stock centrifugal dehydration of step (4), drying is pure to get 5-sulphosalicylic acid
Product.
The refining methd of currently preferred 5-sulphosalicylic acid the following steps are included:
(1) it impregnates, is de- dry: taking 5-sulphosalicylic acid industrial goods, impregnated 10-24 hours with ethyl acetate, 5- sulfosalisylic
The mass ratio of sour industrial goods and ethyl acetate is 1:0.1-0.2, centrifuge dripping 10-20 minutes, obtains immersion material；
(2) material is washed, takes off and does: ethyl acetate being added into the resulting immersion material of step (1), impregnates material and ethyl acetate
Mass ratio be 1:0.05-0.1, centrifuge dripping 10-20 minutes, obtain drying material；
(3) it dissolves, filter: deionized water being added into the resulting drying material of step (2), dry material and deionized water
Mass ratio be 1:0.5-1.5, make dry material sufficiently dissolve, obtain lysate, then into gained lysate be added lysate weight
The active carbon for measuring 0.05-0.7%, after stirring 30-45min at 45-55 DEG C, 4 layers of filter bag natural filtration obtain filter material；
(4) it is concentrated, crystallizes: the resulting filter material of step (3) is concentrated under reduced pressure, be concentrated under reduced pressure 30-65 DEG C of temperature, concentration
To the deionized water for the 80-90% for distilling out deionized water weight added by step (3), obtained concentrate, placement ambient temperature overnight,
Crystallisation by cooling obtains crystallized stock；(5) it is dehydrated, is dry: by step (4) resulting crystallized stock centrifugal dehydration 10-20 minutes, 55-
65 DEG C dry 2-8 hours to get 5-sulphosalicylic acid sterling.
The mass ratio of 5-sulphosalicylic acid industrial goods and ethyl acetate is 8:1 in the preferred step (1).
The mass ratio that material and ethyl acetate are impregnated in the preferred step (2) is 14.2:1.
Drying material and the mass ratio of deionized water are 1.1:1 in the preferred step (3).
88% deionization for distilling out deionized water weight added by step (3) is concentrated into the preferred step (4)
Water, obtained concentrate.
Reduced pressure temperature in the preferred step (4) is to be gradually warmed up program.More preferably it is gradually warmed up program
Start temperature control is concentrated at 30-35 DEG C, and temperature is increased after stablizing to 65 DEG C of concentrations.
The refining methd of 5-sulphosalicylic acid of the present invention the utility model has the advantages that
1. products obtained therefrom quality of the present invention is stablized, indices reach U.S.'s ACS standard.
2. operation of the present invention simple flow, quality is stablized, and is suitble to industrialized production.
Specific embodiment
The refining methd of embodiment 1:5- sulfosalicylic acid is made of following steps:
(1) it impregnates, is de- dry: taking 5-sulphosalicylic acid industrial goods 600g to set in 2L beaker, the second of 60g is added while stirring
Acetoacetic ester impregnates 24 hours, centrifuge dripping 20 minutes, obtains immersion material；
(2) material is washed, takes off and does: being uniformly added into ethyl acetate 35g into the resulting immersion material of step (1), after placing 2min,
It is centrifuged 18min, obtains drying material；
(3) it dissolves, filter: 50-55 DEG C of the deionized water of 900g being added into the resulting drying material of step (2), stirs
Mixing, which makes to dry material, sufficiently dissolves, and lysate is obtained, then the active carbon of lysate weight 5g is added into gained lysate, in 45-
After stirring 30min at 55 DEG C, four layers of filter bag natural filtration obtain filter material；
(4) it is concentrated, crystallizes: the resulting filter material of step (3) is concentrated under reduced pressure, be concentrated under reduced pressure 60-65 DEG C of temperature, concentration
To 790g deionized water (having a large amount of crystal to be precipitated at this time) is distilled out, obtained concentrate pours into material in beaker while hot, puts
Ambient temperature overnight, crystallisation by cooling are set, crystallized stock is obtained；
(5) be dehydrated, be dry: the resulting crystallized stock of step (4) is centrifuged 10-20 minutes, 65 DEG C of dryings 3 hours to get
The 5-sulphosalicylic acid sterling 487g that purity is 99.6%, yield 81.2%, other Testing index meet the mark of U.S. ACS
It is quasi-.
The refining methd of embodiment 2:5- sulfosalicylic acid is made of following steps:
(1) it impregnates, is de- dry: taking 5-sulphosalicylic acid industrial goods 100kg to set in 500L reaction kettle, be added while stirring
The ethyl acetate of 20kg impregnates 24 hours, centrifuge dripping 20 minutes, obtains immersion material；
(2) material is washed, takes off and does: being uniformly added into ethyl acetate 5kg into the resulting immersion material of step (1), after placing 2min,
It is centrifuged 20min, obtains drying material；
(3) it dissolves, filter: 50-55 DEG C of the deionized water of 60kg being added into the resulting drying material of step (2), stirs
Mixing, which makes to dry material, sufficiently dissolves, and obtains lysate, then the active carbon of lysate weight 300g is added into gained lysate,
After stirring 30min at 45-55 DEG C, four layers of filter bag natural filtration obtain filter material；
(4) it is concentrated, crystallizes: the resulting filter material of step (3) is concentrated under reduced pressure, 30-65 DEG C of temperature is concentrated under reduced pressure, and (one opens
The control of beginning temperature divides ethyl acetate bumping slug at 30-35 DEG C with preventing portion, and temperature is increased after stablizing to 65 DEG C), it is concentrated into
52kg deionized water (there are a large amount of crystal to be precipitated at this time) is distilled out, obtained concentrate pours into material in beaker while hot, places
Ambient temperature overnight, crystallisation by cooling, obtain crystallized stock；
(5) be dehydrated, be dry: the resulting crystallized stock of step (4) is centrifuged 10-20 minutes, 65 DEG C of dryings 2 hours to get
The 5-sulphosalicylic acid sterling 85kg that purity is 99.5%, yield 85%, other indexs meet the standard of U.S. ACS.
The refining methd of embodiment 3:5- sulfosalicylic acid is made of following steps:
(1) it impregnates, is de- dry: taking 5-sulphosalicylic acid industrial goods 25kg to set in 500L reaction kettle, be added while stirring
The ethyl acetate of 6.25kg impregnates 20 hours, centrifuge dripping 20 minutes, obtains immersion material；
(2) material is washed, takes off and does: being uniformly added into ethyl acetate 3.55kg into the resulting immersion material of step (1), places 2min
Afterwards, it is centrifuged 20min, obtains drying material；
(3) it dissolves, filter: 50-55 DEG C of the deionized water of 36kg being added into the resulting drying material of step (2), stirs
Mixing, which makes to dry material, sufficiently dissolves, and obtains lysate, then the active carbon of lysate weight 240g is added into gained lysate,
After stirring 30min at 45-55 DEG C, four layers of filter bag natural filtration obtain filter material；
(4) it is concentrated, crystallizes: the resulting filter material of step (3) is concentrated under reduced pressure, 30-65 DEG C of temperature is concentrated under reduced pressure, and (one opens
The control of beginning temperature divides ethyl acetate bumping slug at 30-35 DEG C with preventing portion, and temperature is increased after stablizing to 65 DEG C), it is concentrated into
31.5kg deionized water (there are a large amount of crystal to be precipitated at this time) is distilled out, obtained concentrate pours into material in beaker while hot, puts
Ambient temperature overnight, crystallisation by cooling are set, crystallized stock is obtained；
(5) be dehydrated, be dry: the resulting crystallized stock of step (4) is centrifuged 10-20 minutes, 65 DEG C drying 2.5 hours, i.e.,
The 5-sulphosalicylic acid sterling 21.2kg that purity is 99.7%, yield 84.4% are obtained, every Testing index meets U.S. ACS
Standard.
Comparative example 1: in order to confirm the method for the present invention raw material proportioning amount ranges purification 5-sulphosalicylic acid than other
Ratio range have preferable effect, carry out the refining methd of following 5-sulphosalicylic acid comparative example experiment, this method by with
Lower step is made:
(1) it impregnates, is de- dry: taking 5-sulphosalicylic acid industrial goods 250g to set in 500ML beaker, 60g is added while stirring
Ethyl acetate impregnate 5 hours, centrifuge dripping 20 minutes, obtain immersion material；
(2) material is washed, takes off and does: being uniformly added into ethyl acetate 5g into the resulting immersion material of step (1), after placing 2min,
It is centrifuged 20min, obtains drying material；
(3) it dissolves, filter: 50-55 DEG C of the deionized water of 160g being added into the resulting drying material of step (2), stirs
Mixing, which makes to dry material, sufficiently dissolves, and lysate is obtained, then the active carbon of lysate weight 1g is added into gained lysate, in 45-
After stirring 30min at 55 DEG C, four layers of filter bag natural filtration obtain filter material；
(4) it is concentrated, crystallizes: the resulting filter material of step (3) being concentrated under reduced pressure, 65 DEG C of temperature is concentrated under reduced pressure, is concentrated into
140g deionized water (there are a large amount of crystal to be precipitated at this time) is distilled out, obtained concentrate pours into material in beaker while hot, places
Ambient temperature overnight, crystallisation by cooling, obtain crystallized stock；
(5) be dehydrated, be dry: the resulting crystallized stock of step (4) is centrifuged 10-20 minutes, 65 DEG C drying 2.5 hours, i.e.,
Obtain the 5-sulphosalicylic acid sterling 110g that purity is 98.7%, yield 44%.
Test example: following detection is carried out according to U.S.'s ACS standard to the sample of embodiment preparation, concrete outcome see the table below
1. finished product of table according to U.S.'s ACS standard testing result
From the above experimental results, the purity of the 5-sulphosalicylic acid of embodiment 1-3 purification is obviously refined than comparative example 1
5-sulphosalicylic acid it is high, and the yield of 5-sulphosalicylic acid is only 44% in comparative example 1, well below the receipts of embodiment 1-3
Rate.In addition salicylic acid in finished product, iron, lead index be above standard specified value, illustrate the raw material proportioning range in exquisite method,
Directly affect the properties of product of 5-sulphosalicylic acid.The better performances of 5-sulphosalicylic acid of the method for the present invention preparation, high income,
Impurity content is low.
Claims (8)
1. a kind of refining methd of 5-sulphosalicylic acid, which is characterized in that method includes the following steps:
(1) it impregnates, is de- dry: taking 5-sulphosalicylic acid industrial goods, impregnated with ethyl acetate, centrifuge dripping obtains immersion material；
(2) material is washed, takes off and does: ethyl acetate is added into the resulting immersion material of step (1), centrifuge dripping obtains drying material；
(3) it dissolves, filter: deionized water is added into the resulting drying material of step (2), dissolve drying material sufficiently, obtain
Lysate, then active carbon is added into gained lysate, stirring, filtering obtain filter material；
(4) it is concentrated, crystallizes: the resulting filter material of step (3) is concentrated, obtained concentrate places room temperature, crystallisation by cooling, obtains
Crystallized stock；
(5) it is dehydrated, is dry: by the resulting crystallized stock centrifugal dehydration of step (4), drying to get 5-sulphosalicylic acid sterling.
2. the refining methd of 5-sulphosalicylic acid according to claim 1, which is characterized in that this method includes following step
It is rapid:
(1) it impregnates, is de- dry: taking 5-sulphosalicylic acid industrial goods, impregnated 10-24 hours with ethyl acetate, 5-sulphosalicylic acid work
The mass ratio of industry product and ethyl acetate is 1:0.1-0.2, centrifuge dripping 10-20 minutes, obtains immersion material；
(2) material is washed, takes off and does: ethyl acetate being added into the resulting immersion material of step (1), impregnates the matter of material and ethyl acetate
Amount centrifuge dripping 10-20 minutes, obtains drying material than being 1:0.05-0.1；
(3) it dissolves, filter: deionized water being added into the resulting drying material of step (2), dry the matter of material and deionized water
Amount dissolves drying material sufficiently, obtains lysate, then lysate weight is added into gained lysate than being 1:0.5-1.5
The active carbon of 0.05-0.7%, after stirring 30-45min at 45-55 DEG C, 4 layers of filter bag natural filtration obtain filter material；
(4) it is concentrated, crystallizes: the resulting filter material of step (3) being concentrated under reduced pressure, 30-65 DEG C of temperature is concentrated under reduced pressure, is concentrated into steaming
The deionized water of the 80-90% of deionized water weight added by step (3) is distillated, obtained concentrate places ambient temperature overnight, cooling
Crystallization, obtains crystallized stock；
(5) be dehydrated, be dry: by step (4) resulting crystallized stock centrifugal dehydration 10-20 minutes, 55-65 DEG C it is 2-8 hours dry,
Up to 5-sulphosalicylic acid sterling.
3. the refining methd of 5-sulphosalicylic acid according to claim 2, which is characterized in that 5- sulphur in the step (1)
The mass ratio of base salicylic acid industrial goods and ethyl acetate is 8:1.
4. the refining methd of 5-sulphosalicylic acid according to claim 2, which is characterized in that impregnated in the step (2)
The mass ratio of material and ethyl acetate is 14.2:1.
5. the refining methd of 5-sulphosalicylic acid according to claim 2, which is characterized in that drying in the step (3)
Material and the mass ratio of deionized water are 1.1:1.
6. the refining methd of 5-sulphosalicylic acid according to claim 2, which is characterized in that concentration in the step (4)
To 88% deionized water for distilling out deionized water weight added by step (3), obtained concentrate.
7. the refining methd of 5-sulphosalicylic acid according to claim 1-6, which is characterized in that the step
(4) the reduced pressure temperature in is to be gradually warmed up program.
8. the refining methd of 5-sulphosalicylic acid according to claim 7, which is characterized in that the program that is gradually warmed up is
Start temperature control is concentrated at 30-35 DEG C, and temperature is increased after stablizing to 65 DEG C of concentrations.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| WO2001005754A1 (en) * | 1999-07-15 | 2001-01-25 | Sanofi-Synthelabo | Method for the preparation of 2-methoxy-4-(n-t-butylamino-carbonyl)-benzenesulfonyl chloride |
| CN102219716A (en) * | 2011-04-15 | 2011-10-19 | 太仓沪试试剂有限公司 | Method for purifying 5-sulfosalicylic acid |
| CN103274971A (en) * | 2013-06-19 | 2013-09-04 | 太仓沪试试剂有限公司 | Purification method of 5-sulfosalicylic acid |
-
2018
- 2018-04-12 CN CN201810325931.7A patent/CN110372548A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| WO2001005754A1 (en) * | 1999-07-15 | 2001-01-25 | Sanofi-Synthelabo | Method for the preparation of 2-methoxy-4-(n-t-butylamino-carbonyl)-benzenesulfonyl chloride |
| CN102219716A (en) * | 2011-04-15 | 2011-10-19 | 太仓沪试试剂有限公司 | Method for purifying 5-sulfosalicylic acid |
| CN103274971A (en) * | 2013-06-19 | 2013-09-04 | 太仓沪试试剂有限公司 | Purification method of 5-sulfosalicylic acid |
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Application publication date: 20191025 |