CN114082216A - Efficient evaporation crystallization method of calcium formate - Google Patents
Efficient evaporation crystallization method of calcium formate Download PDFInfo
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- CN114082216A CN114082216A CN202111403141.4A CN202111403141A CN114082216A CN 114082216 A CN114082216 A CN 114082216A CN 202111403141 A CN202111403141 A CN 202111403141A CN 114082216 A CN114082216 A CN 114082216A
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- Prior art keywords
- calcium formate
- evaporation
- crystals
- crystallization method
- crystallization
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- CBOCVOKPQGJKKJ-UHFFFAOYSA-L Calcium formate Chemical compound [Ca+2].[O-]C=O.[O-]C=O CBOCVOKPQGJKKJ-UHFFFAOYSA-L 0.000 title claims abstract description 67
- 239000004281 calcium formate Substances 0.000 title claims abstract description 67
- 229940044172 calcium formate Drugs 0.000 title claims abstract description 67
- 235000019255 calcium formate Nutrition 0.000 title claims abstract description 67
- 238000001704 evaporation Methods 0.000 title claims abstract description 51
- 230000008020 evaporation Effects 0.000 title claims abstract description 46
- 238000002425 crystallisation Methods 0.000 title claims abstract description 45
- 239000007788 liquid Substances 0.000 claims abstract description 40
- 230000008025 crystallization Effects 0.000 claims abstract description 25
- 239000013078 crystal Substances 0.000 claims abstract description 20
- 238000001914 filtration Methods 0.000 claims abstract description 20
- 230000018044 dehydration Effects 0.000 claims abstract description 11
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 11
- 238000000926 separation method Methods 0.000 claims abstract description 8
- 238000009833 condensation Methods 0.000 claims description 25
- 230000005494 condensation Effects 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000007787 solid Substances 0.000 claims description 10
- 239000012535 impurity Substances 0.000 claims description 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 5
- 229910052791 calcium Inorganic materials 0.000 claims description 5
- 239000011575 calcium Substances 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 229920006395 saturated elastomer Polymers 0.000 claims description 5
- 239000002893 slag Substances 0.000 claims description 5
- 238000004062 sedimentation Methods 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000011160 research Methods 0.000 abstract description 2
- 238000001035 drying Methods 0.000 description 12
- 239000000047 product Substances 0.000 description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 4
- 239000012141 concentrate Substances 0.000 description 4
- 238000004806 packaging method and process Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 3
- 206010012735 Diarrhoea Diseases 0.000 description 2
- 239000003674 animal food additive Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000001530 fumaric acid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 2
- 230000017260 vegetative to reproductive phase transition of meristem Effects 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- BCZXFFBUYPCTSJ-UHFFFAOYSA-L Calcium propionate Chemical compound [Ca+2].CCC([O-])=O.CCC([O-])=O BCZXFFBUYPCTSJ-UHFFFAOYSA-L 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000004330 calcium propionate Substances 0.000 description 1
- 235000010331 calcium propionate Nutrition 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0018—Evaporation of components of the mixture to be separated
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/0082—Regulation; Control
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/26—Multiple-effect evaporating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
- B01D36/04—Combinations of filters with settling tanks
- B01D36/045—Combination of filters with centrifugal separation devices
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/13—Crystalline forms, e.g. polymorphs
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention discloses a high-efficiency evaporation crystallization method of calcium formate, which is characterized in that the optimal evaporation rate is selected to obtain calcium formate crystals by controlling the evaporation rate to compare with the crystallization condition, and novel evaporation crystallization equipment used in the high-efficiency evaporation crystallization method of calcium formate comprises a triple-effect evaporation crystallizer for controlling crystallization and a horizontal screw centrifuge for solid-liquid separation which are sequentially connected. The high-efficiency evaporation crystallization method of calcium formate sequentially comprises 3 steps of plate-frame filtration, multi-stage dehydration of a triple-effect evaporation crystallizer and solid-liquid separation of a horizontal screw centrifuge. The invention researches a high-efficiency evaporation crystallization technology of calcium formate, mainly by controlling evaporation rate to compare crystallization conditions, the temperature difference between the front and the back of a film is small, the natural crystallization rate is slow, more crystals are obtained at one time, and the crystallized crystals are larger, so that the most calcium formate crystals are obtained by selecting the optimal evaporation rate.
Description
Technical Field
The invention belongs to the technical field of chemical production, and particularly relates to a high-efficiency evaporation crystallization method of calcium formate.
Background
Calcium formate, also known as calcium formate, is a calcium salt containing formic acid, is used as a novel feed additive newly developed in China, has wide application, can be used as an acidulant to replace citric acid and fumaric acid, and can be widely applied to industrial production of food, chemical industry, building materials and the like. In recent years, calcium formate serving as a novel feed additive can be used as an acid agent to replace citric acid and fumaric acid, can also be used as a preservative and a mildew preventive to replace calcium propionate, is used in various animal feeds, and has the functions of preventing diarrhea and diarrhea, helping digestion and absorption of the feeds and the like. Because the calcium formate product has excellent performance and low price, the calcium formate product has good market at home and abroad at present and has wide sale prospect.
In the prior art, no matter which method is adopted to synthesize calcium formate, the calcium formate solution needs to be prepared into a calcium formate solid product through evaporation, concentration and crystallization treatment, the treatment process not only has high energy consumption, but also may leave other impurities in the solution in the calcium formate solid, thereby affecting the purity of the product. In the prior art, single-effect evaporative crystallization equipment is adopted in evaporative concentration crystallization steps, and the equipment has the disadvantages of high energy consumption, high distilled water discharge amount, high distilled water and condensed water discharge temperature, serious heat energy loss, low heat energy utilization rate, high cooling water consumption for treating distilled water and high environmental protection prevention and control cost in the production process, and becomes a bottleneck for restricting production.
Disclosure of Invention
The invention provides a high-efficiency evaporation crystallization method of calcium formate, aiming at overcoming the defects in the prior art.
The invention is realized by the following technical scheme: the invention discloses a high-efficiency evaporation crystallization method of calcium formate, which is characterized in that the optimal evaporation rate is selected to obtain calcium formate crystals by controlling the evaporation rate to compare with the crystallization condition.
The method for efficiently evaporating and crystallizing the calcium formate specifically comprises the following steps:
(1) and (3) filtering:
filtering the trihydroxy condensation liquid by a plate frame, wherein the filtering temperature is set to be 40-50 ℃ and is used for removing calcium slag and solid impurities in the trihydroxy condensation liquid;
(2) multi-stage dehydration:
the filtered trihydroxy condensation liquid is dehydrated in multiple stages by using a triple-effect evaporation crystallizer, a first-effect evaporator removes part of water in the trihydroxy condensation liquid, a second-effect evaporator concentrates the trihydroxy condensation liquid to a saturated state, and a triple-effect evaporator controls calcium formate crystallization to separate out calcium formate crystals with the mass percent of 80-90%;
(3) centrifuging:
discharging the material from the triple-effect evaporator to a horizontal screw centrifuge for solid-liquid separation, and separating out 8-12% by mass of calcium formate from the liquid in a settling process;
(4) and (3) drying:
washing the solid separated by the horizontal screw centrifuge with water, and drying by using a fluidized bed;
(5) packaging:
and bagging the finished product after fluidized bed drying according to the specification according to the order requirement.
In the method for efficiently evaporating and crystallizing calcium formate of the present invention, the filtration temperature of the filtration in the step (1) is preferably set to 45 ℃.
And (3) carrying out multistage dehydration in the step (2), controlling the optimal evaporation speed of the triple-effect evaporator to be 1.8-2.2 m high flowering each hour, controlling the optimal evaporation speed of the triple-effect evaporator to be 2m high flowering each hour, and controlling calcium formate crystals by the triple-effect evaporator to separate out the crystals from 85% calcium formate in percentage by mass.
And (4) in the centrifugation in the step (3), the liquid enters a sedimentation process, and calcium formate with the mass percentage of 10% is separated.
The invention has the beneficial effects that: the invention researches a calcium formate efficient evaporation crystallization technology, and the calcium formate efficient evaporation crystallization method disclosed by the invention mainly controls the evaporation rate to compare with the crystallization condition, so that the optimal evaporation rate is selected to obtain calcium formate crystals. The evaporation rate and the crystallization rate are both in great relation with the temperature difference, and if a constant temperature film is arranged in the middle, the slower the evaporation rate is, the lower the temperature difference between the front and the back of the film is proved, the natural crystallization rate is also slow, more crystals are crystallized at one time, and the larger the crystals are. Similarly, the faster the evaporation rate, the greater the temperature difference before and after the film, the faster the crystallization rate, and the less disposable crystals.
Detailed Description
The present invention will be described in detail with reference to specific embodiments.
Example 1: the invention discloses a high-efficiency evaporation crystallization method of calcium formate, which is characterized in that the optimal evaporation rate is selected to obtain calcium formate crystals by controlling the evaporation rate to compare with the crystallization condition.
The method for efficiently evaporating and crystallizing the calcium formate specifically comprises the following steps: (1) and (3) filtering: filtering the trihydroxy condensation liquid by a plate frame, wherein the filtering temperature is set to 45 ℃ and is used for removing calcium slag and solid impurities in the trihydroxy condensation liquid; (2) multi-stage dehydration: the filtered trihydroxy condensation liquid is dehydrated in multiple stages by using a triple-effect evaporation crystallizer, a first-effect evaporator removes part of water in the trihydroxy condensation liquid, a second-effect evaporator concentrates the trihydroxy condensation liquid to a saturated state, and a triple-effect evaporator controls calcium formate crystallization to separate out calcium formate crystals with the mass percentage of 85%; controlling the optimal evaporation speed of the triple effect evaporator to be 1.8 m/h, and controlling the optimal evaporation speed of the triple effect evaporator to be 2 m/h; (3) centrifuging: discharging the material from the triple-effect evaporator to a horizontal screw centrifuge for solid-liquid separation, and separating out 10% by mass of calcium formate from the liquid in a settling process; (4) and (3) drying: washing the solid separated by the horizontal screw centrifuge with water, and drying by using a fluidized bed; (5) packaging: and bagging the finished product after fluidized bed drying according to the specification according to the order requirement.
Example 2: the invention discloses a high-efficiency evaporation crystallization method of calcium formate, which specifically comprises the following steps: (1) and (3) filtering: filtering the trihydroxy condensation liquid by a plate frame, wherein the filtering temperature is set to 40 ℃ and is used for removing calcium slag and solid impurities in the trihydroxy condensation liquid; (2) multi-stage dehydration: the filtered trihydroxy condensation liquid is dehydrated in multiple stages by using a triple-effect evaporation crystallizer, a first-effect evaporator removes part of water in the trihydroxy condensation liquid, a second-effect evaporator concentrates the trihydroxy condensation liquid to a saturated state, and a triple-effect evaporator controls calcium formate crystallization to separate out calcium formate crystals with the mass percentage of 80%; (3) centrifuging: discharging the material from the triple-effect evaporator to a horizontal screw centrifuge for solid-liquid separation, and allowing the liquid to enter a settling process to separate calcium formate with the mass percent of 8%; (4) and (3) drying: washing the solid separated by the horizontal screw centrifuge with water, and drying by using a fluidized bed; (5) packaging: and bagging the finished product after fluidized bed drying according to the specification according to the order requirement.
Example 3: the invention discloses a high-efficiency evaporation crystallization method of calcium formate, which specifically comprises the following steps: (1) and (3) filtering: filtering the trihydroxy condensation liquid by a plate frame, wherein the filtering temperature is set to 50 ℃ and is used for removing calcium slag and solid impurities in the trihydroxy condensation liquid; (2) multi-stage dehydration: the filtered trihydroxy condensation liquid is dehydrated in multiple stages by using a triple-effect evaporation crystallizer, a first-effect evaporator removes part of water in the trihydroxy condensation liquid, a second-effect evaporator concentrates the trihydroxy condensation liquid to a saturated state, and a triple-effect evaporator controls calcium formate crystallization to separate out 90% of calcium formate in percentage by mass; (3) centrifuging: discharging the material from the triple-effect evaporator to a horizontal screw centrifuge for solid-liquid separation, and allowing the liquid to enter a sedimentation process to separate calcium formate with the mass percentage of 12%; (4) and (3) drying: washing the solid separated by the horizontal screw centrifuge with water, and drying by using a fluidized bed; (5) and (3) packaging: and bagging the finished product after fluidized bed drying according to the specification according to the order requirement.
In the three examples, by comparing the effects, the effect is remarkably improved when the calcium formate is precipitated and crystallized in the mass percent of 82% in example 1 and the calcium formate is precipitated and crystallized in the mass percent of 83% in example 3 compared with the prior art. The evaporation crystallization effect in example 2 is the best, and the calcium formate crystallization is controlled by the triple-effect evaporator, so that 85% by mass of calcium formate is precipitated and crystallized.
Finally, it should be noted that the above-mentioned contents are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, and that the simple modifications or equivalent substitutions of the technical solutions of the present invention by those of ordinary skill in the art can be made without departing from the spirit and scope of the technical solutions of the present invention.
Claims (7)
1. A method for efficiently evaporating and crystallizing calcium formate is characterized by comprising the following steps: the calcium formate efficient evaporative crystallization method is characterized in that the optimal evaporation rate is selected to obtain calcium formate crystals by controlling the evaporation rate to compare with the crystallization condition, and novel evaporative crystallization equipment used in the calcium formate efficient evaporative crystallization method comprises a triple-effect evaporative crystallizer for controlling crystallization and a horizontal screw centrifuge for solid-liquid separation, which are sequentially connected.
2. The efficient evaporation crystallization method for calcium formate according to claim 1, characterized by: the method for efficiently evaporating and crystallizing the calcium formate comprises the following steps:
(1) and (3) filtering:
filtering the trihydroxy condensation liquid by a plate frame, wherein the filtering temperature is set to be 40-50 ℃ and is used for removing calcium slag and solid impurities in the trihydroxy condensation liquid;
(2) multi-stage dehydration:
multi-stage dehydration is carried out on the filtered trihydroxy condensation liquid by using a triple-effect evaporation crystallizer, part of water in the trihydroxy condensation liquid is removed by using a triple-effect evaporator, the trihydroxy condensation liquid is concentrated to a saturated state by using a double-effect evaporator, calcium formate crystals are controlled by using a single-effect evaporator, and the calcium formate crystals with the mass percentage of 80-90% are all separated out;
(3) centrifuging:
discharging the material from the first-effect evaporator to a horizontal screw centrifuge for solid-liquid separation, and separating out calcium formate with the mass percent of 8-12% by entering the liquid into a settling process.
3. The efficient evaporative crystallization method for calcium formate according to claim 2, characterized by comprising the following steps: in the filtration in the step (1), the filtration temperature was set to 45 ℃.
4. The efficient evaporative crystallization method for calcium formate according to claim 2 or 3, characterized by comprising the following steps: and (3) performing multistage dehydration in the step (2), and controlling the evaporation speed of the triple-effect evaporator to be 1.8-2.2 m cultivation by year/h.
5. The efficient evaporative crystallization method for calcium formate according to claim 4, characterized by comprising the following steps: and (3) in the multi-stage dehydration in the step (2), controlling the evaporation speed of the double-effect evaporator to be 2.4 m/h.
6. The efficient evaporative crystallization method for calcium formate according to claim 4, characterized by comprising the following steps: and (3) in the multi-stage dehydration in the step (2), controlling the calcium formate crystals by using a one-effect evaporator to separate out the crystals from 85% by mass of calcium formate.
7. The efficient evaporative crystallization method for calcium formate according to claim 2, characterized by comprising the following steps: and (4) in the centrifugation in the step (3), the liquid enters a sedimentation process, and calcium formate with the mass percentage of 10% is separated.
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CN202111403141.4A CN114082216A (en) | 2021-11-24 | 2021-11-24 | Efficient evaporation crystallization method of calcium formate |
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CN202111403141.4A CN114082216A (en) | 2021-11-24 | 2021-11-24 | Efficient evaporation crystallization method of calcium formate |
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CN202111403141.4A Pending CN114082216A (en) | 2021-11-24 | 2021-11-24 | Efficient evaporation crystallization method of calcium formate |
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103113208A (en) * | 2013-02-27 | 2013-05-22 | 天津大学 | Continuous production process for preparing calcium formate through calcium hydroxide carbonylation |
CN104208902A (en) * | 2014-09-28 | 2014-12-17 | 湖北吉星化工集团有限责任公司 | Triple-effect evaporation and crystallization production process and device |
US20200048128A1 (en) * | 2018-08-08 | 2020-02-13 | Aquatech International, Llc | Method and Apparatus for Gasification Wastewater Treatment |
CN111362492A (en) * | 2018-12-26 | 2020-07-03 | 广州市迈源科技有限公司 | Double-effect MVR evaporation treatment method |
-
2021
- 2021-11-24 CN CN202111403141.4A patent/CN114082216A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103113208A (en) * | 2013-02-27 | 2013-05-22 | 天津大学 | Continuous production process for preparing calcium formate through calcium hydroxide carbonylation |
CN104208902A (en) * | 2014-09-28 | 2014-12-17 | 湖北吉星化工集团有限责任公司 | Triple-effect evaporation and crystallization production process and device |
US20200048128A1 (en) * | 2018-08-08 | 2020-02-13 | Aquatech International, Llc | Method and Apparatus for Gasification Wastewater Treatment |
CN111362492A (en) * | 2018-12-26 | 2020-07-03 | 广州市迈源科技有限公司 | Double-effect MVR evaporation treatment method |
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Application publication date: 20220225 |