CN106146564B - A kind of preparation method of the L sodium antimony tartrates of high yield pulp1 - Google Patents
A kind of preparation method of the L sodium antimony tartrates of high yield pulp1 Download PDFInfo
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- CN106146564B CN106146564B CN201610587717.XA CN201610587717A CN106146564B CN 106146564 B CN106146564 B CN 106146564B CN 201610587717 A CN201610587717 A CN 201610587717A CN 106146564 B CN106146564 B CN 106146564B
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- sodium
- tartaric acid
- antimony
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- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- AFWAHDXCIBPFNW-UHFFFAOYSA-J sodium;antimony(3+);2,3-dihydroxybutanedioate Chemical class [Na+].[Sb+3].[O-]C(=O)C(O)C(O)C([O-])=O.[O-]C(=O)C(O)C(O)C([O-])=O AFWAHDXCIBPFNW-UHFFFAOYSA-J 0.000 title abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 239000007787 solid Substances 0.000 claims abstract description 16
- 229910000410 antimony oxide Inorganic materials 0.000 claims abstract description 14
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000706 filtrate Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 4
- 239000000047 product Substances 0.000 claims abstract description 4
- CXKXLTJUIOMDHK-OLXYHTOASA-N [Na].[Sb].C([C@H](O)[C@@H](O)C(=O)O)(=O)O Chemical compound [Na].[Sb].C([C@H](O)[C@@H](O)C(=O)O)(=O)O CXKXLTJUIOMDHK-OLXYHTOASA-N 0.000 claims description 19
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 13
- 239000011734 sodium Substances 0.000 claims description 13
- 229910052708 sodium Inorganic materials 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 8
- 229910052785 arsenic Inorganic materials 0.000 claims description 7
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 239000012141 concentrate Substances 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims description 2
- BMUJWLXKZUCOEI-UHFFFAOYSA-N antimony sodium Chemical compound [Na].[Sb] BMUJWLXKZUCOEI-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- NKAAEMMYHLFEFN-UHFFFAOYSA-M monosodium tartrate Chemical class [Na+].OC(=O)C(O)C(O)C([O-])=O NKAAEMMYHLFEFN-UHFFFAOYSA-M 0.000 abstract 1
- 239000003153 chemical reaction reagent Substances 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- 235000019441 ethanol Nutrition 0.000 description 6
- 238000012360 testing method Methods 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 125000005909 ethyl alcohol group Chemical group 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- LAOOXBLMIJHMFO-UHFFFAOYSA-N 1-[2-(diethylamino)ethylamino]-4-methylthioxanthen-9-one;hydron;chloride Chemical compound Cl.S1C2=CC=CC=C2C(=O)C2=C1C(C)=CC=C2NCCN(CC)CC LAOOXBLMIJHMFO-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000001843 schistosomicidal effect Effects 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 235000019605 sweet taste sensations Nutrition 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/90—Antimony compounds
- C07F9/902—Compounds without antimony-carbon linkages
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/90—Antimony compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Disclosed herein is a kind of preparation method of L sodium antimony tartrates, first L sodium hydrogen tartrates are dissolved by heating into deionized water, after solution is heated to 80 DEG C ~ 90 DEG C of temperature, antimony oxide solid powder is added portionwise, it is stirring while adding, continue to react 2 ~ 6h under fluidized state after adding, then filter, filtrate heating is concentrated into 1.5 ~ 1.7g/mL of density（70℃~90℃）, room temperature is naturally cooled to, the solution by portions after cooling is added in absolute ethyl alcohol, it is stirring while adding, that is, there are a kind of a large amount of white sodium antimony tartrate solids of L to separate out, through centrifuging, L sodium antimony tartrate finished products are obtained after drying.The preparation method steady qualities of L sodium antimony tartrates provided by the present invention, purity are high, a yield up to more than 98%, it is easy to operate, be adapted to industrialized production.
Description
Technical field
The invention belongs to chemical reagent preparation field, and in particular to a kind of preparation side of the L-TARTARIC ACID antimony sodium of high yield pulp1
Method.
Background technology
L-TARTARIC ACID antimony sodium is a kind of white solid powder.Band sweet taste, moisture absorption is poisonous, is dissolved in water, insoluble in ethanol, water
Solution is in acidity.The mordant and treatment Schistosomicide being mainly used as in weaving and leather industry.The synthesis of sodium antimony tartrate
In theory and uncomplicated, available data generates L-TARTARIC ACID antimony sodium using L-TARTARIC ACID hydrogen sodium and antimony oxide reaction more, but
It is that L-TARTARIC ACID antimony sodium Synthesis liquid can not obtain finished product by the method directly concentrated, although it is decomposed without obvious at high temperature
Phenomenon, but after Synthesis liquid is concentrated, obtains the suspension body of similar pasty state, crystal can not be also obtained even in refrigerator cold-storage 24h.
Data in terms of the preparation of the L-TARTARIC ACID antimony sodium of document report is seldom, and Zhang Jiuzhi is sent out on 1958 pharmacy circular
The table preparation method of L-TARTARIC ACID antimony sodium, disclose and added using 96% ethanol in filtrate, L-TARTARIC ACID antimony sodium can be separated out
Crystal, but 500~600ml 96% ethanol need to be consumed by preparing 100g samples, and yield only has 80%.And existing market
On antimony tartrate sodium reagent content below 98%.
The content of the invention
For overcome the deficiencies in the prior art, it is an object of the invention to provide a kind of L-TARTARIC ACID antimony sodium of high yield pulp1
Preparation method.
To reach above-mentioned purpose, the present invention is achieved by the following technical solutions.
A kind of preparation method of the L-TARTARIC ACID antimony sodium of high yield pulp1, comprises the following steps：
(1) L-TARTARIC ACID hydrogen sodium is added in deionized water, dissolves by heating, treat that solution is heated to 80 DEG C~90 DEG C of temperature
When, antimony oxide solid powder is slowly added in batches, it is stirring while adding, continue to react 2~6h under fluidized state after adding,
Then filter；
(2) concentration step：Filtrate heating evaporation is concentrated, 1.5~1.7g/ of solution density when being concentrated to 70 DEG C~90 DEG C
ML, then naturally cool to room temperature；
(3) crystallisation step：Solution by portions after cooling is added in absolute ethyl alcohol, it is stirring while adding, that is, have a large amount of white
Color L-TARTARIC ACID antimony sodium solid is separated out, and through centrifuging, L-TARTARIC ACID antimony sodium finished product is obtained after drying.Through de- after ethanol recovery used
It is reusable after water, distillation.
Further in the step (1), the mass ratio of L-TARTARIC ACID hydrogen sodium and deionized water is 1:5~10.
Antimony oxide quality is further added according to the content of arsenic in antimony oxide in the step (1)
0.01%~0.05% vulcanized sodium.
Powdered active carbon drainage is added when further being filtered in the step (1), the addition of activated carbon is every
20~100g of 100L solution.The characteristics of chemical reagent, requires that the clarity of filtrate will reach certain standard, but filtrate meeting sometimes
There is fluorescence phenomenon, if though can solve problem using the filter plant filtering of high precision, equipment cost significantly increases therewith
Add, and the micro substance that may be introduced into filter material, this is not permitted in chemical reagent production；But add in the solution
The appearance of fluorescence is just avoided that using the filter bag of 3~6 layers of common chemical fibre material after a small amount of activated carbon, that is, greatly reduces cost
The reagent needs of reagent production are met again.
Further in the step (3), the volume ratio of concentrate and absolute ethyl alcohol after cooling is 1:0.5~2.
Further drying temperature control is at 80~120 DEG C, 6~10h of drying time in the step (3), per 2h stirrings
Once.
Beneficial effect：Compared with prior art, the advantage of the invention is that：
1) involved solvent be deionized water and absolute ethyl alcohol in the present invention, cheap and easy to get, and can be recycled, operation
Simplicity, safety and environmental protection, it is adapted to industrialized production.
2) yield of L-TARTARIC ACID antimony sodium prepared in the present invention is more than 98%, and steady quality, purity is more than 98.5%,
Other indexs are satisfied by the standard of chemical reagent, can meet domestic medicine, requirement of the chemical enterprise to L-TARTARIC ACID antimony sodium.
Embodiment
With reference to example, the present invention is described in further detail.
Embodiment 1
Weigh 200g L-TARTARIC ACID hydrogen sodium to be slowly added into 1500mL deionized waters, heat while stirring, treat completely molten
Xie Hou, continue heated solution to 90 DEG C, 160g antimony oxide solids are then added portionwise, it is stirring while adding.Antimony oxide
Continue to react 2h under boil condition after adding, 0.016g vulcanized sodium (being made into the aqueous solution) arsenic removal, stirring are added after reacting completely
Filtered after 20min with filter paper, the filtrate measure clarity after filtering, heated after qualified and be concentrated to density 1.70g/mL (70 DEG C),
Room temperature is naturally cooled to, 300ml absolute ethyl alcohols is measured and pours into beaker, be slowly added to concentrate, it is stirring while adding, that is, separate out big
Measure white L-TARTARIC ACID antimony sodium solid, after centrifuging 10min, by solid in 80 DEG C of drys 10h, obtaining sample 333g, (theoretical calculation is answered
This obtains 338.9g), yield 98.25%, censorship purity is 98.6%, and all other indexs are satisfied by the mark of chemical reagent
Standard, specific testing result are shown in Table 1.
Embodiment 2
Weigh 300g L-TARTARIC ACID hydrogen sodium to be slowly added into 3000mL deionized waters, heat while stirring, treat completely molten
Xie Hou, continue heated solution to 80 DEG C, 240g antimony oxide solids are then added portionwise, it is stirring while adding.Antimony oxide
Continue to react 6h under boil condition after adding, 0.1g vulcanized sodium (being made into the aqueous solution) arsenic removal, stirring are added after reacting completely
Filtered after 20min with filter paper, the filtrate measure clarity after filtering, heated after qualified and be concentrated to density 1.50g/mL (90 DEG C),
Room temperature is naturally cooled to, 400ml absolute ethyl alcohols is measured and pours into beaker, be slowly added to concentrate, it is stirring while adding, that is, separate out big
White solid is measured, after centrifuging 10min, by solid in 120 DEG C of dry 6h, obtaining sample 501g, (theoretical calculation should obtain
508.4g), yield 98.54%, censorship purity are 98.9%, and all other indexs are satisfied by the standard of chemical reagent, specifically
Testing result is shown in Table 2.
Table 2
| Sequence number | Detection project | Unit | Standard setting | Measured value |
| 1 | Content (NaSbC4H4O7) | W/ % | ≥98.0 | 98.9 |
| 2 | Clarity test | It is qualified | It is qualified | |
| 3 | Arsenic (As) | W/ % | ≤0.002 | 0.002 |
| 4 | Heavy metal (in terms of Pb) | W/ % | ≤0.001 | 0.001 |
| 5 | Loss on drying | W/ % | ≤2.0 | 0.1 |
Embodiment 3
Deionized water 165kg is added into reactor, L-TARTARIC ACID hydrogen sodium 33kg is then added portionwise, steam is opened and adds
Heat, until completely dissolved, continue heated solution to 90 DEG C, 25kg antimony oxide solids are then added portionwise, it is stirring while adding.
Antimony oxide continues to react 4h under boil condition after adding, and 12.5g vulcanized sodium (being made into the aqueous solution) is added after reacting completely
Arsenic removal, four layers of sock filtration are used after stirring 20min, filtrate after filtering determines clarity, unqualified, adds 150g activated carbons again
Filtering, after gained filtrate clarity is qualified, heating is concentrated to density 1.60g/mL (85 DEG C), then naturally cools to room temperature, then
Absolute ethyl alcohol 40kg is added in another reactor, the concentrate after cooling is added portionwise in absolute ethyl alcohol, it is stirring while adding,
Separate out a large amount of white solids, after centrifuging 20min, by solid in 110 DEG C of dry 7h, obtaining sample 51.9kg, (theoretical calculation should
Obtain 52.9kg), yield 98.1%, censorship purity is 98.8%, and all other indexs are satisfied by the standard of chemical reagent, tool
Physical examination is surveyed and the results are shown in Table 3.
Table 3
| Sequence number | Detection project | Unit | Standard setting | Measured value |
| 1 | Content (NaSbC4H4O7) | W/ % | ≥98.0 | 98.8 |
| 2 | Clarity test | It is qualified | It is qualified | |
| 3 | Arsenic (As) | W/ % | ≤0.002 | 0.002 |
| 4 | Heavy metal (in terms of Pb) | W/ % | ≤0.001 | 0.001 |
| 5 | Loss on drying | W/ % | ≤2.0 | 0.1 |
The present invention is illustrated according to above-described embodiment, it will be appreciated that above-described embodiment does not limit this in any form
Invention, all technical schemes obtained using equivalent substitution or equivalent transformation mode, is within the scope of the present invention.
Claims (3)
1. the preparation method of the L-TARTARIC ACID antimony sodium of a kind of high yield pulp1, it is characterised in that comprise the following steps：
（1）L-TARTARIC ACID hydrogen sodium is added in deionized water, dissolved by heating, when solution is heated to 80 DEG C ~ 90 DEG C of temperature, in batches
Antimony oxide solid powder is added, it is stirring while adding, continue to react 2 ~ 6h under fluidized state after adding, then filter；
（2）Concentration step：Filtrate heating evaporation is concentrated, 1.5 ~ 1.7g/mL of solution density when being concentrated into 70 DEG C ~ 90 DEG C, then
Naturally cool to room temperature；
（3）Crystallisation step：Solution after cooling is added in absolute ethyl alcohol, it is stirring while adding, that is, there are a large amount of white L- winestones
Sour antimony sodium solid is separated out, and through centrifuging, L-TARTARIC ACID antimony sodium finished product, the step are obtained after drying（1）In, L-TARTARIC ACID hydrogen sodium is with going
The mass ratio of ionized water is 1:5 ~ 10, the step（1）The middle content according to arsenic in antimony oxide, add antimony oxide matter
The vulcanized sodium of amount 0.01% ~ 0.05%；
The step（3）In, the volume ratio of concentrate and absolute ethyl alcohol after cooling is 1:0.5~2.
A kind of 2. preparation method of the L-TARTARIC ACID antimony sodium of high yield pulp1 according to claim 1, it is characterised in that the step
Suddenly（1）Powdered active carbon drainage is added during middle filtering, the addition of activated carbon is per 20 ~ 100g of 100L solution.
A kind of 3. preparation method of the L-TARTARIC ACID antimony sodium of high yield pulp1 according to claim 1, it is characterised in that the step
Suddenly（3）Middle drying temperature control is at 80 ~ 120 DEG C, 6 ~ 10h of drying time, per 2h stirrings once.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610587717.XA CN106146564B (en) | 2016-07-25 | 2016-07-25 | A kind of preparation method of the L sodium antimony tartrates of high yield pulp1 |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610587717.XA CN106146564B (en) | 2016-07-25 | 2016-07-25 | A kind of preparation method of the L sodium antimony tartrates of high yield pulp1 |
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| Publication Number | Publication Date |
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| CN106146564A CN106146564A (en) | 2016-11-23 |
| CN106146564B true CN106146564B (en) | 2018-02-09 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| DE4339841A1 (en) * | 1993-11-23 | 1995-05-24 | Basf Magnetics Gmbh | Finely divided needle-like magnetic chromium di:oxide |
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