CN113020094A - Method and device for automatically washing purple uric acid - Google Patents
Method and device for automatically washing purple uric acid Download PDFInfo
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- CN113020094A CN113020094A CN202110223914.4A CN202110223914A CN113020094A CN 113020094 A CN113020094 A CN 113020094A CN 202110223914 A CN202110223914 A CN 202110223914A CN 113020094 A CN113020094 A CN 113020094A
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- 238000005406 washing Methods 0.000 title claims abstract description 139
- 238000000034 method Methods 0.000 title claims abstract description 26
- LEHOTFFKMJEONL-UHFFFAOYSA-N Uric Acid Chemical compound N1C(=O)NC(=O)C2=C1NC(=O)N2 LEHOTFFKMJEONL-UHFFFAOYSA-N 0.000 title claims description 29
- TVWHNULVHGKJHS-UHFFFAOYSA-N Uric acid Natural products N1C(=O)NC(=O)C2NC(=O)NC21 TVWHNULVHGKJHS-UHFFFAOYSA-N 0.000 title claims description 29
- 229940116269 uric acid Drugs 0.000 title claims description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 67
- 239000000706 filtrate Substances 0.000 claims abstract description 38
- 239000000463 material Substances 0.000 claims abstract description 36
- VQTZGUYEOZNKQH-UHFFFAOYSA-N 5-[(2,4,6-trioxo-1,3-diazinan-5-yl)imino]-1,3-diazinane-2,4,6-trione Chemical compound O=C1NC(=O)NC(=O)C1N=C1C(=O)NC(=O)NC1=O VQTZGUYEOZNKQH-UHFFFAOYSA-N 0.000 claims abstract 17
- 238000003756 stirring Methods 0.000 claims description 33
- 238000003825 pressing Methods 0.000 claims description 27
- 239000002904 solvent Substances 0.000 claims description 27
- HRRVLSKRYVIEPR-UHFFFAOYSA-N 6-hydroxy-5-nitroso-1H-pyrimidine-2,4-dione Chemical compound OC1=NC(O)=C(N=O)C(O)=N1 HRRVLSKRYVIEPR-UHFFFAOYSA-N 0.000 claims description 17
- 238000010009 beating Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- 239000008213 purified water Substances 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 2
- 229960001763 zinc sulfate Drugs 0.000 claims description 2
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 13
- 238000005984 hydrogenation reaction Methods 0.000 abstract description 9
- 239000003960 organic solvent Substances 0.000 abstract description 5
- 238000004140 cleaning Methods 0.000 abstract description 2
- 238000004537 pulping Methods 0.000 description 16
- RYYVLZVUVIJVGH-UHFFFAOYSA-N caffeine Chemical compound CN1C(=O)N(C)C(=O)C2=C1N=CN2C RYYVLZVUVIJVGH-UHFFFAOYSA-N 0.000 description 15
- 238000006722 reduction reaction Methods 0.000 description 8
- 238000001514 detection method Methods 0.000 description 7
- LPHGQDQBBGAPDZ-UHFFFAOYSA-N Isocaffeine Natural products CN1C(=O)N(C)C(=O)C2=C1N(C)C=N2 LPHGQDQBBGAPDZ-UHFFFAOYSA-N 0.000 description 6
- 229960001948 caffeine Drugs 0.000 description 6
- VJEONQKOZGKCAK-UHFFFAOYSA-N caffeine Natural products CN1C(=O)N(C)C(=O)C2=C1C=CN2C VJEONQKOZGKCAK-UHFFFAOYSA-N 0.000 description 6
- 239000000047 product Substances 0.000 description 5
- MLIREBYILWEBDM-UHFFFAOYSA-N cyanoacetic acid Chemical compound OC(=O)CC#N MLIREBYILWEBDM-UHFFFAOYSA-N 0.000 description 4
- 238000012544 monitoring process Methods 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 3
- 239000000543 intermediate Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- MGJKQDOBUOMPEZ-UHFFFAOYSA-N N,N'-dimethylurea Chemical compound CNC(=O)NC MGJKQDOBUOMPEZ-UHFFFAOYSA-N 0.000 description 2
- -1 carboxylic acid compound Chemical class 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- VNDYJBBGRKZCSX-UHFFFAOYSA-L zinc bromide Chemical compound Br[Zn]Br VNDYJBBGRKZCSX-UHFFFAOYSA-L 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000000413 hydrolysate Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000009935 nitrosation Effects 0.000 description 1
- 238000007034 nitrosation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006798 ring closing metathesis reaction Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
- 229940102001 zinc bromide Drugs 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B13/00—Accessories or details of general applicability for machines or apparatus for cleaning
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/102—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration with means for agitating the liquid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/14—Removing waste, e.g. labels, from cleaning liquid
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D239/00—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings
- C07D239/02—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings
- C07D239/24—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members
- C07D239/28—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, directly attached to ring carbon atoms
- C07D239/46—Two or more oxygen, sulphur or nitrogen atoms
- C07D239/60—Three or more oxygen or sulfur atoms
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Processing Of Solid Wastes (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
本发明提供了一种紫脲酸自动洗涤的方法，根据紫脲酸含量或紫脲酸溶料后的滤液pH对物料进行分类洗涤；本发明还提供了一种实现紫脲酸自动洗涤的装置；本发明解决了传统水洗紫脲酸仅可去除紫脲酸中水溶性杂质的难题，减轻了紫脲酸所带杂质对后续加氢还原的影响；实现了紫脲酸的分类、分等级清洗，减少有机溶剂及洗涤水用量。
The invention provides a method for automatic washing of purpuric acid, which is to classify and wash materials according to the content of purpuric acid or the pH of the filtrate after the purpuric acid is dissolved; the invention also provides a device for automatic washing of purpuric acid The invention solves the problem that the traditional washing of purpuric acid can only remove water-soluble impurities in purpuric acid, reduces the influence of impurities carried by purpuric acid on subsequent hydrogenation reduction, and realizes the classification and graded cleaning of purpuric acid. , reduce the amount of organic solvents and washing water.
Description
Technical Field
The invention belongs to the field of chemical pharmacy, and particularly relates to a method and a device for automatically washing purple uric acid.
Background
The caffeine synthesis process using cyanoacetic acid and dimethyl urea as starting materials becomes a mainstream production process of caffeine series products due to the advantages of simple process, high yield, good stability of intermediates and the like. The purple uric acid is generated by carrying out ring closure and nitrosation on dimethyl urea and cyanoacetic acid, is an important intermediate for producing caffeine series products, and the content and impurity level of the purple uric acid directly influence the subsequent hydrogenation reduction reaction, thereby influencing the yield and quality of the caffeine series products. How to reduce the impurity level in the reaction system before the hydrogenation reduction becomes an important factor in improving the yield of caffeine product quality.
At present, in order to reduce the influence of the violuric acid on a nickel catalyst in a hydrogenation reduction system, water-soluble impurities in the violuric acid are washed away mainly by adopting a clean water washing mode, but organic impurities in the violuric acid cannot be effectively removed, researches prove that part of the organic impurities in the violuric acid can be hydrolyzed under an alkaline condition, a hydrolysate and a subsequent intermediate dimethyl-FAU are condensed to form rings, and the ring is heated, dehydrogenated, aromatized and hydrolyzed under the catalysis of residual nickel in the presence of illumination and oxygen to generate a carboxylic acid compound under the presence of subsequent alkali and acid, so that the quality of a caffeine finished product is seriously influenced.
The patent (CN101812024B) discloses a purification method of dimethyl violuric acid, which specifically adopts alcohol, ether or ketone organic solvent to mix with water and adds soluble zinc salt to wash the violuric acid, and can increase the content of the violuric acid from 60% to more than 90%, but the disclosed method stays in the laboratory research stage, and organic solvents such as methanol, tert-butyl alcohol and acetone used in the disclosed method can be remained in caffeine, so that organic impurities in the finished caffeine exceed the standard, and the introduction of halogen elements such as zinc chloride and zinc bromide can also affect impurity systems, which obviously has a great risk to the caffeine with dual attributes of medicine and food. The washed purple uric acid still has 10 percent of impurities, and the residual impurities still can influence the subsequent hydrogenation reduction reaction.
Disclosure of Invention
The invention provides a method for automatically washing purple uric acid, which classifies and washes materials according to the content of the purple uric acid or the pH of filtrate after the purple uric acid is dissolved:
(1) washing by the first method when the content of the purple uric acid is more than 95% (w/w) or the pH of a filtrate obtained by dispersing the purple uric acid in purified water is more than 4;
(2) washing by the second method when the content of the purple uric acid is less than or equal to 95% (w/w) and the pH of the filtrate obtained by dispersing the purple uric acid in purified water is less than or equal to 4.
The first method comprises the following washing steps:
(1) mixing purple uric acid: water is mixed according to the mass ratio of 1: 3, dispersing the dissolved materials in a material dissolving tank V1, stirring for 10-15 minutes until the materials are uniformly dispersed, pressing the materials to a washing tank V2-1 by using compressed air, stirring for 10 minutes, then opening the washing tank V2-1 to compress the air, and pressing 2/3 washing water;
(2) after the pressure is finished, adding water into a washing tank V2-1 to the original volume, stirring for 10 minutes, then starting compressed air, and pressing 2/3 washing water out to a filtrate collection tank V4-1;
(3) after the pressure is finished, adding water into a washing tank V2-1 to the original volume, stirring for 10 minutes, then starting compressed air, and pressing 2/3 washing water out to a filtrate washing tank V4-1;
(4) and monitoring the pH value of the washing water for the third time, if the pH value is more than 6.5, finishing the washing, adding water into the material in the washing tank V2-1 to supplement the volume to the original volume, and transferring the material to a pulping tank V3-1 for pulping for later use.
The second method comprises the following washing steps:
(1) mixing purple uric acid: water is mixed according to the mass ratio of 1: 2, dispersing the dissolved materials in a material dissolving tank V1, stirring for 10-15 minutes until the materials are uniformly dispersed, pressing the materials to a washing tank V2-2 by using compressed air, stirring for 10 minutes, then opening the washing tank V2-2 to compress the air, and pressing 1/2 washing water to a filtrate collecting tank V4-1;
(2) adding the solvent in the auxiliary solvent tank V5-1 and the saline solution in the auxiliary solvent tank V5-2 into a washing tank V2-2, complementing the volume of the raw material, stirring for 15 minutes, then starting compressed air, and pressing 3/4 washing liquid into a filtrate collecting tank V4-2;
(3) after the pressure is finished, adding water into a washing tank V2-2 until the volume of the raw dissolved material is 1.5 times, stirring for 10 minutes, then starting compressed air, and pressing 2/3 washing water out to a filtrate washing tank V4-2;
(4) after the pressure is finished, adding water into a washing tank V2-2 to 1.5 times of the volume of the original dissolved material, stirring for 10 minutes, then starting compressed air, and pressing 2/3 washing water out to a filtrate washing tank V4-1;
(5) and monitoring the pH value of the fifth washing water, finishing the washing if the pH value is more than 6.5, adding water into the material in the washing tank V2-2 to make up to 1.5 times of the volume of the original dissolved material, and transferring the material to a pulping tank V3-2 for pulping for later use.
The invention also provides a device for realizing the automatic washing of the purple uric acid, which comprises 1 solvent tank V1, 2 washing tanks V2-1 and V2-2, 2 beating tanks V3-1 and V3-2, 2 filtrate collection tanks V4-1 and V4-2, and 2 auxiliary solvent tanks V5-1 and V5-2; the solvent tank V1 is connected with a washing tank V2-1 and a washing tank V2-2, the washing tank V2-1 is connected with a pulping tank V3-1, the washing tank V2-1 is connected with a filtrate collecting tank V4-1, the washing tank V2-2 is connected with the pulping tank V3-2, the pulping tank V3-2 is connected with the filtrate collecting tanks V4-1 and V4-2, and the auxiliary solvent tanks V5-1 and V5-2 are respectively connected with the washing tank V2-2.
All tank bodies of the purple uric acid automatic washing device are provided with liquid level meters, the dissolving tank, the washing tank and the pulping tank are respectively provided with double-layer stirring, the washing tank is provided with a pressure gauge, a pH monitoring meter is arranged on a connecting pipeline of the washing tank and the filtrate collecting tank, and the pH monitoring meter, the pressure gauge and a liquid level counting value can be automatically controlled through PLC control.
The solvent in the auxiliary solvent tank V5-1 is ethanol with the volume fraction of more than 99 percent;
the saturated aqueous solution of the salt solution zinc sulfate in the auxiliary solvent tank V5-2.
The method solves the problem that the water-soluble impurities in the conventional water-washed uric acid can only be removed, and reduces the influence of the impurities carried by the uric acid on the subsequent hydrogenation reduction; the classification and grading cleaning of the purple uric acid are realized, and the use amount of an organic solvent and washing water is reduced; salts and organic solvents suitable for the washing of violuric acid are also identified.
Drawings
FIG. 1 is a schematic view of an automatic washing process of violuric acid, wherein: v1 is a dissolving tank, V2-1 and V2-2 are washing tanks, V3-1 and V3-2 are beating tanks, V4-1 and V4-2 are filtrate collection tanks, V5-1 and V5-2 are auxiliary solvent tanks, liquid level meters (L1, L2-1, L2-2, L3-1, L3-2, L4-1, L4-2), double-layer stirring (M1, M2-1, M2-2, M3-1, M3-2), pH monitors (pH-1, pH-2), pressure meters (P2-1 and P2-2).
Detailed Description
The following further description, without limiting the scope of the invention, with reference to the accompanying drawings, specific embodiments are as follows:
example 1:
through detection, the absolute content of the purple uric acid is 96.21 percent, the first ground washing method is adopted for washing, 500kg of the purple uric acid is put into a material dissolving tank V1, adding 1500L of water dispersible dissolving material, stirring for 13 min, pressing the material to a washing tank V2-1 with compressed air, stirring for 10 min, then opening the washing tank V2-1 to compress air, pressing out 1000L of water, then adding 1000L of water into the washing tank V2-1, stirring for 10 min, then opening the compressed air, pressing out 1000L of washing water to a filtrate collecting tank V4-1, then adding 1000L of water into the washing tank V2-1 again, stirring for 10 min, then opening the compressed air, pressing out 1000L of washing water to a filtrate collecting tank V4-1, detecting the pH of the third washing water to be 6.75, finishing the washing, 1000L of water is added into the washing tank V2-1, and the materials are transferred to the pulping tank V3-1 to be pulped for standby. The violuric acid in the pulping tank V3-1 is taken, filtered, dried and then subjected to absolute content detection, the detection result is 99.85%, and the washed violuric acid is used for hydrogenation reduction reaction, and the yield is 97.82%.
Example 2:
detecting that the absolute content of the purple uric acid is 94.85 percent, taking 100g of the purple uric acid to disperse in 300mL of water, detecting that the pH of filtrate is 4.23, washing by adopting a first washing method, putting 500kg of the purple uric acid into a material dissolving tank V1, adding 1500L of water dispersing and dissolving material, stirring for 12 minutes, pressing the material to a washing tank V2-1 by using compressed air to wash, stirring for 10 minutes, then opening the washing tank V2-1 to compress the compressed air, pressing out 1000L of water, adding 1000L of water into the washing tank V2-1, stirring for 10 minutes, then opening the compressed air, pressing out 1000L of washing water to a filtrate collecting tank V4-1, then adding 1000L of water into the washing tank V2-1 again, stirring for 10 minutes, then opening the compressed air, pressing out 1000L of washing water to a filtrate collecting tank V4-1, detecting that the pH of the washing water for the third time is 6.83, after the washing is finished, adding 1000L of water into the washing tank V2-1, and transferring the materials to a pulping tank V3-1 for pulping for standby. The violuric acid in the pulping tank V3-1 is taken, filtered, dried and then subjected to absolute content detection, the detection result is 99.65%, and the washed violuric acid is used for hydrogenation reduction reaction, and the yield is 96.92%.
Example 3:
detecting that the absolute content of the purple uric acid is 93.68%, dispersing 100g of the purple uric acid in 300mL of water, measuring the pH of the filtrate to be 4.02, washing by adopting a second washing method, putting 500kg of the purple uric acid into a solution tank V1, adding 1000L of water dispersion solution, stirring for 15 minutes, pressing the materials to a washing tank V2-2 by using compressed air, washing for 10 minutes, opening the washing tank V2-2 by using compressed air, pressing 500L of washing water to a filtrate collecting tank V4-1, adding 300L of a solvent in an auxiliary solvent tank V5-1 and 200L of a saline solution in the auxiliary solvent tank V5-2 to the washing tank V2-2, stirring for 15 minutes, then opening the compressed air, pressing 750L of the washing water to the filtrate collecting tank V4-2, then adding 1250L of water to the washing tank V2-2, stirring for 10 minutes, opening the compressed air, pressing 1000L of the washing water to the filtrate washing tank V4-2, adding 1000L of water into the washing tank V2-2, stirring for 10 min, then starting compressed air, pressing out 1000L of washing water to the filtrate washing tank V4-1, detecting the pH of the fifth washing water to be 6.78, after washing, adding 1000L of water into the washing tank V2-2, transferring the material to the pulping tank V3-2, and pulping for later use. The violuric acid in the pulping tank V3-2 is taken, filtered, dried and then subjected to absolute content detection, the detection result is 99.72%, and the washed violuric acid is used for hydrogenation reduction reaction, and the yield is 97.03%.
Claims (6)
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| CN202110223914.4A CN113020094B (en) | 2021-03-01 | 2021-03-01 | Method and device for automatic washing of violuric acid |
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| CN202110223914.4A CN113020094B (en) | 2021-03-01 | 2021-03-01 | Method and device for automatic washing of violuric acid |
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2021
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| CN107602310A (en) * | 2017-10-30 | 2018-01-19 | 西安近代化学研究所 | Acid elution method is driven in a kind of gas whistle formula serialization suitable for explosive |
| CN109761208A (en) * | 2019-03-06 | 2019-05-17 | 深圳海纳百川科技有限公司 | A kind of technique and device of ferric phosphate washing |
| CN215480665U (en) * | 2021-03-01 | 2022-01-11 | 山东新华制药股份有限公司 | Automatic washing device of purple uric acid |
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