CN103159637B - A kind of method promoting industrial disodium ethylene diamine tetraacetate quality - Google Patents
A kind of method promoting industrial disodium ethylene diamine tetraacetate quality Download PDFInfo
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- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 title claims abstract description 54
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 24
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 title claims abstract 14
- 230000001737 promoting effect Effects 0.000 title abstract description 7
- 238000002425 crystallisation Methods 0.000 claims abstract description 29
- 230000008025 crystallization Effects 0.000 claims abstract description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000012452 mother liquor Substances 0.000 claims abstract description 10
- 210000004243 sweat Anatomy 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000012498 ultrapure water Substances 0.000 claims abstract description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 7
- 238000006073 displacement reaction Methods 0.000 claims abstract description 3
- 230000008020 evaporation Effects 0.000 claims abstract 2
- 238000001704 evaporation Methods 0.000 claims abstract 2
- 239000007787 solid Substances 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 6
- BDOYKFSQFYNPKF-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(carboxymethyl)amino]acetic acid;sodium Chemical compound [Na].[Na].OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O BDOYKFSQFYNPKF-UHFFFAOYSA-N 0.000 claims description 4
- SMEGJBVQLJJKKX-HOTMZDKISA-N [(2R,3S,4S,5R,6R)-5-acetyloxy-3,4,6-trihydroxyoxan-2-yl]methyl acetate Chemical compound CC(=O)OC[C@@H]1[C@H]([C@@H]([C@H]([C@@H](O1)O)OC(=O)C)O)O SMEGJBVQLJJKKX-HOTMZDKISA-N 0.000 claims description 4
- 229940081735 acetylcellulose Drugs 0.000 claims description 4
- 229920002301 cellulose acetate Polymers 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 239000012982 microporous membrane Substances 0.000 claims description 4
- 230000035900 sweating Effects 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 238000001914 filtration Methods 0.000 abstract description 6
- 239000000706 filtrate Substances 0.000 abstract description 5
- 239000000546 pharmaceutical excipient Substances 0.000 abstract description 4
- 229940124531 pharmaceutical excipient Drugs 0.000 abstract description 4
- 238000012360 testing method Methods 0.000 abstract description 4
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 42
- 239000000243 solution Substances 0.000 description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 229910021645 metal ion Inorganic materials 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 238000005352 clarification Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- -1 plumbous Chemical compound 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical compound CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- KXZJHVJKXJLBKO-UHFFFAOYSA-N chembl1408157 Chemical compound N=1C2=CC=CC=C2C(C(=O)O)=CC=1C1=CC=C(O)C=C1 KXZJHVJKXJLBKO-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000536 complexating effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229920002545 silicone oil Polymers 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003146 anticoagulant agent Substances 0.000 description 1
- 229940127219 anticoagulant drug Drugs 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
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- 230000007812 deficiency Effects 0.000 description 1
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- 239000003814 drug Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 229960001484 edetic acid Drugs 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- LTYRAPJYLUPLCI-UHFFFAOYSA-N glycolonitrile Chemical compound OCC#N LTYRAPJYLUPLCI-UHFFFAOYSA-N 0.000 description 1
- 239000008233 hard water Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
- UEUXEKPTXMALOB-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O UEUXEKPTXMALOB-UHFFFAOYSA-J 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of method promoting industrial disodium ethylene diamine tetraacetate quality.With industrial disodium ethylene diamine tetraacetate for raw material, be placed in single tube crystallizer, through high pure nitrogen displacement, multi-step melt crystallization, dissolved by the disodium ethylene diamine tetraacetate high purity water obtained, micro-pore-film filtration, filtrate is through evaporation, crystallization, dry, the disodium ethylene diamine tetraacetate of the quality that namely gets a promotion.After testing, the standard of YY0206-95 " pharmaceutical excipient disodium ethylene diamine tetraacetate " is met.Carry out fusion-crystallization by after the disposing mother liquor in the inventive method, reach the standard of industrial disodium ethylene diamine tetraacetate, also can mix with raw material and reuse, gained sweat also can directly mix with raw material after reclaiming to be reused.
Description
Technical field
The present invention relates to a kind of method promoting industrial disodium ethylene diamine tetraacetate quality, particularly relate to a kind of by multi-step melt crystallization, micro-pore-film filtration removes impurity metal ion, promotes the method for disodium ethylene diamine tetraacetate quality.
Background technology
Disodium ethylene diamine tetraacetate is also known as EDETATE SODIUM, containing two crystal water in disodium ethylene diamine tetraacetate product, it is a kind of excellent complexing agent, for by water softening, many kinds of metal ions in effective complexing hard water, as calcium, magnesium and iron, plumbous, copper, manganese etc., the ability of its complexing many kinds of metal ions and separating metal is quite strong, can be used as bleach-fixing liquid and the dyeing auxiliary of color sensitive material washing processing, fibre finish, cosmetics additive, medicine, food, the micro-fertilizer of agrochemistry is produced, blood anticoagulant, water-softening chemicals in washing composition, stablizer, synthetic rubber, polymerization starter and heavy metal quantitative analysis agent etc.In addition, in styrene-butadiene rubber(SBR) polymerization with in chlorination reduction initiating system, also can be used as the integral part of promoting agent, be mainly used in chelated iron ion, control polymerization rate.
The molecular formula of disodium ethylene diamine tetraacetate is C
10h
14n
2na
2o
82H
2o, structural formula is as follows:
In prior art, the industrial method of disodium ethylene diamine tetraacetate has: 1) sodium cyanide method: add in ethylenediamine solution by the mixture of sodium cyanide and formaldehyde, pass into air under reduced pressure, use vitriol oil adjust ph, through decolouring, filter, concentrated, Crystallization Separation, dry finished product.2) chloroactic acid method: chloroacetic sodium hydroxide solution is mixed, add quadrol respectively, sodium hydroxide solution, will through activated carbon decolorizing, concentrated, filter the filtrate that obtains through crystallization, be separated, the ethylenediamine tetraacetic acid (EDTA) for preparing and sodium hydroxide reacts, dehydration, filtration, neutralization, namely obtain the disodium ethylene diamine tetraacetate of purifying.
Chinese patent CN2009101913637 reports with quadrol and hydroxyacetonitrile as raw material reacts in sodium hydroxide solution, prepare the method for disodium ethylene diamine tetraacetate, but because disodium ethylene diamine tetraacetate is by the impact of initial feed, water quality, and the limitation of production technique, foreign metal ion content in products obtained therefrom is higher, and impurity metal ion etc. are difficult to the desired value reaching disodium ethylene diamine tetraacetate standard.
Yet there are no the relevant report promoting disodium ethylene diamine tetraacetate quality method.
Summary of the invention
Problem to be solved by this invention is to provide a kind of method promoting disodium ethylene diamine tetraacetate quality, to overcome the deficiency that in prior art, disodium ethylene diamine tetraacetate impurity metal ion content is higher.
Technical conceive of the present invention is such:
With industrial disodium ethylene diamine tetraacetate for raw material, be placed in pipe in single tube crystallizer, through multi-step melt crystallization after replacing with high pure nitrogen, obtain the disodium ethylene diamine tetraacetate of fusion-crystallization, dissolve through high purity water, micro-pore-film filtration, steam except moisture content from filtrate, crystallization, drying, the disodium ethylene diamine tetraacetate of the quality that namely gets a promotion.
Specifically, the method for lifting disodium ethylene diamine tetraacetate quality of the present invention, comprises the steps:
(1) industrial disodium ethylene diamine tetraacetate is carried out multi-step melt crystallization as follows in single tube crystallizer:
1. first industrial disodium ethylene diamine tetraacetate is joined in single tube crystallizer in pipe, with high pure nitrogen displacement 2-3 time;
2. super thermostatic oil bath pot is started, progressively heat up with the speed of 5 ~ 6 DEG C/min and be heated to 255 ~ 260 DEG C, after the complete melting of the disodium ethylene diamine tetraacetate in pipe in single tube crystallizer, by the temperature-stable of fused solution in pipe in single tube crystallizer at 253 ~ 255 DEG C, then to make in single tube crystallizer fused solution temperature in pipe be down to 235 ~ 237 DEG C with the rate of temperature fall of 0.4-0.5 DEG C/min to carry out crystallization;
3. fusion-crystallization process 2-3 time is repeated by above-mentioned condition;
4. open dispensing valve and release mother liquor;
5. control the temperature of super thermostatic oil bath pot, make the temperature in single tube crystallizer in pipe rise to 247 ~ 250 DEG C with the temperature rise rate of 0.3-0.5 DEG C/min, carry out sweating operation, open dispensing valve in single tube crystallizer after pipe homo(io)thermism and release sweat;
6. control the temperature of super thermostatic oil bath pot, improve oil bath temperature to 255 ~ 260 DEG C, the solid in crystallizer in pipe is all melted, through discharge, collect, cool the disodium ethylene diamine tetraacetate obtaining multi-step melt crystallization.
Wherein in above-mentioned steps, adopt the temperature of super thermostatic oil bath pot computer heating control oil bath pan, the material of single tube crystallizer is stainless steel, and inner tube diameter is 50mm, and outer tube diameter is 100mm, high 200mm, and upper end is full jacket flange, and lower end is for closing blind plate.
(2) disodium ethylene diamine tetraacetate high purity water step (1) obtained filters with microporous membrane after dissolving.
Wherein, described high purity water be greater than 17M Ω .cm than resistance value, described microporous membrane is the acetyl cellulose film of aperture 0.10-0.22 μm, can through commercially available channel buy obtain.
(3) disodium ethylene diamine tetra-acetic acid solution step (2) obtained steams except moisture content, crystallization, drying, must promote the disodium ethylene diamine tetraacetate of quality.
Wherein, being steam filtering by step (2) disodium ethylene diamine tetra-acetic acid solution obtained at ambient pressure except moisture content, cooling the crystal that obtains at the temperature of 80 ~ 90 DEG C dry 8 ~ 10 hours.
After testing, adopt the disodium ethylene diamine tetraacetate that the inventive method is obtained, meet the standard of YY0206-95 " pharmaceutical excipient disodium ethylene diamine tetraacetate ".
Compared with prior art, the present invention has following advantage:
1) the present invention adopts multi-step melt crystallization, and micro-pore-film filtration membrane separation technique, effectively can remove the impurity metal ion in industrial disodium ethylene diamine tetraacetate, promotes the quality of disodium ethylene diamine tetraacetate.
2) carry out fusion-crystallization by after the disposing mother liquor in the inventive method, can reach the standard of industrial disodium ethylene diamine tetraacetate, also can mix with raw material and reuse, gained sweat also can directly mix with raw material after reclaiming to be reused.
Accompanying drawing explanation
Fig. 1 is the temperature control schema that the present invention promotes disodium ethylene diamine tetraacetate quality method.Wherein 1 is power supply, and 2 is super thermostatic oil bath pot, and 3 is single tube crystallizer, and 4 is nitrogen inlet, and 5 is dispensing valve.
Embodiment
Below by specific embodiment, the present invention is described further, but embodiment does not limit the scope of the invention.It should be noted that, following examples are only in order to illustrate technical scheme of the present invention and unrestricted.Although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that, can modify to the technical scheme of invention or equivalent replacement, and not depart from the scope of technical solution of the present invention, it all should be encompassed in right of the present invention
Embodiment 1
Disodium ethylene diamine tetraacetate 600g is ground to form granular, add pipe in single tube crystallization, under normal temperature, use nitrogen replacement 3 times.Open super thermostatic oil bath, with the heating rate of 5 DEG C/min to 257 DEG C (temperature in experiment is the temperature of thermophore silicone oil in oil bath pan), after the complete melting of device Raw to be crystallized, reduce the temperature to 252 DEG C of single tube crystallizer, after temperature-stable, by the time variable control oil bath temperature of oil bath pan, the fused solution in crystallizer is made to be cooled to 237 DEG C by the speed of 0.5 DEG C/min, repeat this intensification cooling process 2 times, open dispensing valve in device to be crystallized after temperature-stable and release mother liquor.Then progressively oil bath temperature to 247 DEG C is improved with the speed of 0.3 DEG C/min, carry out sweating operation, open dispensing valve in crystallizer after homo(io)thermism and release sweat, again oil bath temperature is risen to 257 DEG C, solid in crystallizer all melted, through discharge, collects, cool the disodium ethylene diamine tetraacetate 500g after obtaining fusion-crystallization, in addition mother liquor cools to obtain solid 60g, and sweat cools to obtain solid 40g.
The high purity water that the above-mentioned disodium ethylene diamine tetraacetate 100g 500ml obtained after fusion-crystallization is greater than 17M Ω .cm than resistance value is dissolved, filter with the acetyl cellulose film that aperture is 0.22 μm under normal temperature, the filtrate normal pressure obtained steams except moisture content, cooling obtains white powder crystallization, be placed in 80 DEG C of baking ovens dry 10 hours, the disodium ethylene diamine tetraacetate 97g of the quality that namely gets a promotion.Carry out detection to this product to analyze, result shows, meets YY0206-95, " pharmaceutical excipient disodium ethylene diamine tetraacetate " standard.Concrete detection data are referring to following table 1.
Table 1
| Test item | Desired value measured value |
| Content is (with C 10H 14N 2Na 2O 8·2H 2O counts), % | ≥99.0%99.7% |
| The color of solution and clarity | Achromaticity and clarification achromaticity and clarification |
| PH value (5% aqueous solution) | 4.0～6.04.5 |
| Muriate (in Cl), % | ≤0.0050.001 |
| Iron (Fe), % | ≤0.0010.0006 |
| Heavy metal (in Pb), % | ≤0.0010.0005 |
| Prussiate | Without the reaction of aobvious prussiate reaction cyanide-free |
Embodiment 2
Disodium ethylene diamine tetraacetate 600g is ground to form granular, add pipe in single tube crystallization, with nitrogen replacement 2 times.Open constant temperature oil bath, be heated to 260 DEG C (temperature in experiment is the temperature of thermophore silicone oil in oil bath pan) with the speed of 6 DEG C/min, after the complete melting of device Raw to be crystallized, reduce the temperature to 250 DEG C of single tube crystallizer, after temperature-stable, by the time variable control oil bath temperature of oil bath pan, the fused solution in crystallizer is made to be cooled to 235 DEG C by the speed of 0.4 DEG C/min, repeat this heating, cooling step 3 time, open dispensing valve in device to be crystallized after temperature-stable and release mother liquor.Then progressively oil bath temperature to 247 DEG C is improved with the speed of 0.5 DEG C/min, carry out sweating operation, open dispensing valve in crystallizer after homo(io)thermism and release sweat, again oil bath temperature is risen to 260 DEG C, solid in crystallizer all melted, through discharge, collects, cool the disodium ethylene diamine tetraacetate 480g after obtaining fusion-crystallization, in addition mother liquor cools to obtain solid 60g, and sweat cools to obtain solid 60g.
The high purity water that the above-mentioned disodium ethylene diamine tetraacetate 100g 1000ml obtained after fusion-crystallization is greater than 17M Ω .cm than resistance value is dissolved, filter with the acetyl cellulose film that aperture is 0.10 μm under normal temperature, the filtrate normal pressure obtained steams except moisture content, cooling obtains white powder crystallization, be placed in 90 DEG C of baking ovens dry 8 hours, the disodium ethylene diamine tetraacetate 96g of the quality that namely gets a promotion.Carry out detection to this product to analyze, result shows, meets YY0206-95 completely, " pharmaceutical excipient disodium ethylene diamine tetraacetate " standard.Concrete detection data are referring to following table 2.
Table 2
| Test item | Desired value | Measured value |
| Content is (with C 10H 14N 2Na 2O 8·2H 2O counts), % | ≥99.0% | 99.8% |
| The color of solution and clarity | Achromaticity and clarification | Achromaticity and clarification |
| PH value (5% aqueous solution) | 4.0～6.0 | 4.8 |
| Muriate (in Cl), % | ≤0.005 | 0.001 |
| Iron (Fe), % | ≤0.001 | 0.0008 |
| Heavy metal (in Pb), % | ≤0.001 | 0.0006 |
| Prussiate | Cyanide-free reacts | Cyanide-free reacts |
Claims (5)
1. promote a method for disodium ethylene diamine tetraacetate quality, it is characterized in that, comprise the steps:
(1) industrial disodium ethylene diamine tetraacetate is placed in single tube crystallizer and carries out multi-step melt crystallization by following program:
1. industrial disodium ethylene diamine tetraacetate is joined in single tube crystallizer in pipe, with high pure nitrogen displacement 2-3 time;
2. start super thermostatic oil bath pot, progressively heat up be heated to 255 ~ 260 DEG C with the speed of 5 ~ 6 DEG C/min, after the complete melting of the disodium ethylene diamine tetraacetate in single tube crystallizer, the temperature controlling pipe in single tube crystallizer is down to 253 ~ 255 DEG C; The fused solution temperature in single tube crystallizer in pipe is made to be down to 235 ~ 237 DEG C with the rate of temperature fall of 0.4-0.5 DEG C/min again;
3. above-mentioned steps 2. fusion-crystallization process 2-3 time is repeated;
4. open dispensing valve and release mother liquor;
5. control the temperature of super thermostatic oil bath pot, make the temperature in single tube crystallizer in pipe rise to 247 ~ 250 DEG C with the temperature rise rate of 0.3-0.5 DEG C/min, carry out sweating operation, open dispensing valve in single tube crystallizer after pipe homo(io)thermism and release sweat;
6. control the temperature of super thermostatic oil bath pot, improve oil bath temperature to 255 ~ 260 DEG C, the solid in crystallizer in pipe is all melted, through discharge, collect, cool, namely obtain the disodium ethylene diamine tetraacetate through multi-step melt crystallization;
(2) filter with microporous membrane after the disodium ethylene diamine tetraacetate obtained through above-mentioned steps (1) being dissolved with high purity water; Described high purity water be greater than 17M Ω cm than resistance value;
(3) the disodium ethylene diamine tetra-acetic acid solution evaporation that will obtain through above-mentioned steps (2), crystallization, drying, obtain target product.
2. method according to claim 1, is characterized in that, in step (1), the material of described single tube crystallizer is stainless steel, and inner tube diameter is 50mm, and outer tube diameter is 100mm, high 200mm, and upper end is full jacket flange, and lower end is for closing blind plate.
3. method according to claim 1, is characterized in that, in step (2), described microporous membrane to be aperture the be acetyl cellulose film of 0.10-0.22 μm, the mass volume ratio of disodium ethylene diamine tetraacetate and high purity water is 0.1 ~ 0.2:1g/ml.
4. method according to claim 1, it is characterized in that, in step (3), the disodium ethylene diamine tetra-acetic acid solution obtained by step (2) is steamed at ambient pressure except moisture content, cooling, crystal at the temperature of 80 ~ 90 DEG C dry 8 ~ 10 hours.
5. method according to claim 1, is characterized in that, after the mother liquor in step (1), sweat reclaim, mother liquor can reach raw material standard after concentrating and carrying out fusion-crystallization, and sweat directly mixes with raw material to be reused.
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| KR100275791B1 (en) * | 1998-06-23 | 2000-12-15 | 박호군 | Method of crystalization of edta4na |
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|---|---|---|---|---|
| CN1944397A (en) * | 2006-10-25 | 2007-04-11 | 四川省天然气化工研究院 | Process for preparing EDTA disodium salt |
| CN101607920A (en) * | 2008-06-19 | 2009-12-23 | 天津市化学试剂研究所 | The preparation method of reference reagent-disodium ethylene diamine tetraacetate |
| CN101723842A (en) * | 2009-11-06 | 2010-06-09 | 重庆紫光鼎福化工有限责任公司 | Method for preparing ethylene diamine tetraacetic acid (EDTA) disodium salt |
| CN102796019A (en) * | 2011-05-26 | 2012-11-28 | 李宽义 | Method for environment-friendly clean production of high-purity ethylene diamine tetraacetic acid (EDTA) |
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