CN106316829B - Four water acetic acid magnesium and its preparation process and application - Google Patents
Four water acetic acid magnesium and its preparation process and application Download PDFInfo
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- CN106316829B CN106316829B CN201610694151.0A CN201610694151A CN106316829B CN 106316829 B CN106316829 B CN 106316829B CN 201610694151 A CN201610694151 A CN 201610694151A CN 106316829 B CN106316829 B CN 106316829B
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- 239000011777 magnesium Substances 0.000 title claims abstract description 51
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 48
- PQLVXDKIJBQVDF-UHFFFAOYSA-N acetic acid;hydrate Chemical compound O.CC(O)=O PQLVXDKIJBQVDF-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- 239000013078 crystal Substances 0.000 claims abstract description 30
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 claims abstract description 23
- 238000001914 filtration Methods 0.000 claims abstract description 21
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 16
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000007664 blowing Methods 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims description 43
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 42
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 229960000583 acetic acid Drugs 0.000 claims description 21
- 239000011654 magnesium acetate Substances 0.000 claims description 20
- 229940069446 magnesium acetate Drugs 0.000 claims description 20
- 235000011285 magnesium acetate Nutrition 0.000 claims description 20
- 239000012362 glacial acetic acid Substances 0.000 claims description 19
- 239000000706 filtrate Substances 0.000 claims description 16
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 13
- 239000012043 crude product Substances 0.000 claims description 12
- 238000002425 crystallisation Methods 0.000 claims description 12
- 239000000395 magnesium oxide Substances 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 11
- 235000011054 acetic acid Nutrition 0.000 claims description 9
- 230000008025 crystallization Effects 0.000 claims description 9
- 150000001243 acetic acids Chemical class 0.000 claims description 8
- 239000012141 concentrate Substances 0.000 claims description 8
- 239000002002 slurry Substances 0.000 claims description 8
- 239000012530 fluid Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 5
- 230000008020 evaporation Effects 0.000 claims description 5
- 235000021050 feed intake Nutrition 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 5
- 239000012452 mother liquor Substances 0.000 claims description 5
- 230000001376 precipitating effect Effects 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 238000004513 sizing Methods 0.000 claims description 5
- 239000003516 soil conditioner Substances 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 3
- 239000000052 vinegar Substances 0.000 claims 1
- 235000021419 vinegar Nutrition 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 15
- 238000004043 dyeing Methods 0.000 abstract description 7
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract description 5
- 239000003054 catalyst Substances 0.000 abstract description 5
- 239000000460 chlorine Substances 0.000 abstract description 5
- 229910052801 chlorine Inorganic materials 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 5
- 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 abstract description 4
- 239000002537 cosmetic Substances 0.000 abstract description 4
- 238000004332 deodorization Methods 0.000 abstract description 4
- YQGOJNYOYNNSMM-UHFFFAOYSA-N eosin Chemical compound [Na+].OC(=O)C1=CC=CC=C1C1=C2C=C(Br)C(=O)C(Br)=C2OC2=C(Br)C(O)=C(Br)C=C21 YQGOJNYOYNNSMM-UHFFFAOYSA-N 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000003755 preservative agent Substances 0.000 abstract description 4
- 230000002335 preservative effect Effects 0.000 abstract description 4
- 239000011734 sodium Substances 0.000 abstract description 4
- 229910052708 sodium Inorganic materials 0.000 abstract description 4
- 230000001954 sterilising effect Effects 0.000 abstract description 4
- 238000004659 sterilization and disinfection Methods 0.000 abstract description 4
- 239000004753 textile Substances 0.000 abstract description 4
- 229910052770 Uranium Inorganic materials 0.000 abstract description 3
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 abstract description 3
- 238000004806 packaging method and process Methods 0.000 abstract 1
- 239000003814 drug Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- GBRRPEMZLIOYBH-UHFFFAOYSA-F [Mg+2].C(C)(=O)[O-].[U+6].C(C)(=O)[O-].C(C)(=O)[O-].C(C)(=O)[O-].C(C)(=O)[O-].C(C)(=O)[O-].C(C)(=O)[O-].C(C)(=O)[O-] Chemical compound [Mg+2].C(C)(=O)[O-].[U+6].C(C)(=O)[O-].C(C)(=O)[O-].C(C)(=O)[O-].C(C)(=O)[O-].C(C)(=O)[O-].C(C)(=O)[O-].C(C)(=O)[O-] GBRRPEMZLIOYBH-UHFFFAOYSA-F 0.000 description 1
- AQBNSUGIFRIQSL-UHFFFAOYSA-N acetyl acetate;magnesium Chemical group [Mg].CC(=O)OC(C)=O AQBNSUGIFRIQSL-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 150000002901 organomagnesium compounds Chemical class 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Classifications
-
- 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
- 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
- C07C53/00—Saturated compounds having only one carboxyl group bound to an acyclic carbon atom or hydrogen
- C07C53/08—Acetic acid
- C07C53/10—Salts thereof
-
- 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)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Cosmetics (AREA)
Abstract
The invention discloses a kind of four water acetic acid magnesium and its preparation process and application, the preparation process to include the following steps：Synthesis, press filtration, concentration, is concentrated, is crystallized, centrifuging blowing, drying, packaging reaction again.Concentration is divided into two parts by preparation process of the present invention, and energy-efficient, simple for process, process is easy to control, and low in raw material price is easy to get, and production cost is relatively low.Four water acetic acid magnesium made of the present invention, appearance white crystal, stay in grade；Molecular formula C4H14O8Mg, molecular weight 214.46, density 0.8g/l, 72 80 DEG C of fusing point；Content 98% or more, in 320 350ppm, pH value relatively stablize, and maintains 79 by chlorine.Four water acetic acid magnesium of the invention are in feed addictive, cosmetics, catalyst and the intermediate of organic synthesis；Uranium acetate magnesium is prepared, to measure sodium；And the application of deodorization, sterilization, preservative, textile dyeing, eosin dyeing, the fixation of nigrosine etc..
Description
Technical field
The present invention relates to four water acetic acid magnesium preparing technical fields, more particularly, to a kind of four water acetic acid magnesium and its preparation process
And application.
Background technology
For a long time, magnesium resource is mainly used to produce refractory material and the lower inorganic chemical product of added value, using model
It encloses relatively narrow.Currently, still having the synthesis and application study that many scientific research institutions are dedicated to organo-magnesium compound.Wherein magnesium acetate is
A kind of important broad sense magnesium metal organic compound.There are two types of states for common magnesium acetate：One is acetic anhydride magnesium, another
It is the four water acetic acid magnesium with the crystallization water.Four water acetic acid magnesium are a kind of metallo-organic compounds being readily synthesized, and purity is high, cost
It is low, there is higher surcharge.Simultaneously as its good water solubility, nontoxic, it is a kind of green chemical products, so greatly
Power develops its application foreground very much.
Chinese magnesium reserves account for the 20% of world's total amount, and common magnesium carbonate, magnesium chloride and magnesia can be in nature
As the base stock of four water acetic acid magnesium of synthesis, furtheing investigate new process conditions has important practical significance.In recent years, four
Many properties of water acetic acid magnesium are causing the concern of people, such as have extensively in chemical industry, material, medicine, agricultural field
Wealthy application prospect.The study found that four water acetic acid magnesium can be widely used as the intermediate of organic synthesis, catalyst, analytical reagent,
Deicing salt, modifying agent etc..But in the intermediate and the application aspects such as feed addictive as organic synthesis, application cost is slightly higher,
Popularization and application are affected, marketing still needs to running a period of time.
Invention content
First technical problem to be solved by this invention is to provide a kind of preparation process of four water acetic acids magnesium, the invention work
Concentration is divided into two parts by skill, and energy-efficient, preparation process is simple, and process is easy to control, and low in raw material price is easy to get, production
Cost is relatively low.
In order to solve above-mentioned first technical problem, the technical solution adopted in the present invention is：
The preparation process of four water acetic acid magnesium, reaction route are as follows：Magnesia is mixed into slurry with water, then anti-with glacial acetic acid
It answers, feed liquid press filtration after reaction removes filter residue；After separation of solid and liquid, filtrate crystallisation obtains magnesium acetate crude product, and drying obtains four
Water acetic acid magnesium finished product.
The preparation process of four water acetic acid magnesium, comprises the following steps that：
(1) it synthesizes：Into the tank of sizing mixing for filling suitable quantity of water, powdery light calcined magnesia is put into, is stirred evenly；Again by slurry with
Glacial acetic acid is put in proportion into synthesis reactor, puts into the molar ratio of light calcined magnesia and glacial acetic acid 1:1.9-2.1；
(2) it reacts：Feed intake end, exothermic heat of reaction, keeps reaction temperature and keeps the temperature；It is pH value in 6-7 to control reaction end,
Baume degrees is between 15-16 ° of B é；
(3) press filtration：By the feed liquid press filtration after reaction, filtrate is obtained；
(4) it concentrates：By filtrate concentration and evaporation between 25-26 ° of B é of Baume degrees；
(5) it concentrates again：Feed liquid is concentrated to Baume degrees between 28-29 ° of B é；
(6) it crystallizes：The feed liquid that will be concentrated to give, is pumped into crystallization kettle；First lead to condensed water and be cooled to 43-46 DEG C, acetic acid is added
Magnesium crystal seed；Feed liquid is waited for begin with crystal precipitation, Temperature fall is to wait for that crystal is grown up；
(7) blowing is centrifuged：After precipitating crystal, crystallization feed liquid is put into centrifuge, mother liquor is detached with crystal, is obtained thick
Product magnesium acetate；
(8) it dries：Crude product magnesium acetate is in 40-60 DEG C of drying of fluid bed；
(9) it packs：The four water acetic acid magnesium finished products that will be obtained, are packed.
In the step (1), the content of magnesia is 80%, and the content of glacial acetic acid is 98%.
It in the step (2), keeps reaction temperature at 80-90 DEG C, keeps the temperature 2-3 hours.
In the step (3), feed liquid press filtration carries out in plate and frame filter press.
In the step (3), the filter residue obtained after feed liquid press filtration is used to prepare soil conditioner.
Concentration in the step (4) is to utilize scraper evaporator, and scraper plate concentration is carried out to filtrate.
Concentrating again in the step (5) is to utilize MVR inspissators, and the feed liquid after being concentrated to scraper evaporator carries out dense
Contracting.
In the step (6), the quantity of magnesium acetate crystal seed is added to be put into according to every square stock liquid 30-45kg.
Second technical problem to be solved by this invention is to provide a kind of four water acetic acid magnesium, is by claim 1 to 9
Any one of described in four water acetic acid magnesium preparation process made by, appearance white crystal, molecular formula C4H14MgO8, molecule
Amount 214.46,72-80 DEG C of fusing point, density 0.8g/l, chlorine in 320-350ppm, 98% or more, relatively stablize content, maintains by pH value
In 7-9.
Third technical problem to be solved by this invention is four water acetic acid magnesium, in feed addictive, cosmetics, catalyst
With the intermediate of organic synthesis；Uranium acetate magnesium is prepared, to measure sodium；And deodorization, sterilization, preservative, textile dyeing,
Eosin dyeing, the application for fixing aspect of nigrosine.
Compared with the prior art the present invention, has the advantages that：
Concentration is divided into two parts in preparation process of the present invention, wherein：One be using scraper evaporator to filtrate into
Row concentration；The other is using MVR inspissators, the feed liquid concentrated to scraper evaporator is concentrated again, energy saving to reach
Efficient purpose.The present invention is simple, and process is easy to control, and low in raw material price is easy to get, and production cost is relatively low.
Utilize four water acetic acid magnesium made of present invention process, appearance white crystal, stay in grade；Molecular formula C4H14O8Mg,
Molecular weight 214.46, density 0.8g/l, 72-80 DEG C of fusing point；Content 98% or more, in 320-350ppm, pH value relatively stablize by chlorine,
Maintain 7-9.
Using four water acetic acid magnesium made of present invention process, it is mainly used for feed addictive, cosmetics, catalyst and organic
The intermediate of synthesis；Uranium acetate magnesium is prepared, to measure sodium；And applied to medicine, industry, deodorization, sterilization, preservative,
Textile dyeing, eosin dyeing, the fixation etc. of nigrosine.
Four water acetic acid magnesium made of present invention process, in application aspect, intermediate, feed addictive as organic synthesis
Deng the speciality of tool organic metal salt, it is easy degradation, it is non-hazardous to biology and environment.Other opposite simple metal salt, application cost
Slightly lower, marketing application effect is good.
Description of the drawings
Fig. 1 is the preparation technology flow chart of four water acetic acid magnesium；
Fig. 2 is the process equipment schematic diagram of four water acetic acid magnesium.
Specific implementation mode
With reference to specific embodiment, the present invention is done and is further described in detail：
Four water acetic acid magnesium preparation processes, reaction route are as follows：
Magnesia is mixed into slurry with water, then is reacted with glacial acetic acid, and feed liquid press filtration after reaction removes filter residue.Solid-liquid
After separation, filtrate crystallisation obtains magnesium acetate crude product, and drying obtains four water acetic acid magnesium finished products.
Equipment used in present invention process has：It sizes mixing tank；5000L synthesis reactors；Plate and frame filter press；Scraper evaporator；MVR
Inspissator；Crystallization kettle；Centrifuge；Fluid bed, electronic scale.
Raw material used in present invention process has：The magnesia of content 80%, the glacial acetic acid of content 98%.
Embodiment 1
(1) it synthesizes：Into the tank of sizing mixing for filling suitable quantity of water, powdery light calcined magnesia 390kg is put into, is stirred evenly.Again will
Slurry opens stirring with glacial acetic acid 794kg input synthesis reactors.Wherein：The molar ratio of input light calcined magnesia and glacial acetic acid exists
1:1.9.The content of magnesia is 80%, and the content of glacial acetic acid is 98%.
(2) it reacts：Feed intake end, exothermic heat of reaction, is maintained at 80-90 DEG C of reaction temperature, keeps the temperature 2-3 hours.Control is anti-
Answer terminal be pH value in 6-7, Baume degrees is between 15-16 ° of B é.
(3) press filtration：By the feed liquid after reaction through plate and frame filter press press filtration, filtrate is obtained.Obtained filter residue after press filtration is used
In preparing soil conditioner.
(4) scraper evaporator concentrates：Using scraper evaporator, by filtrate concentration and evaporation between 25-26 ° of B é of Baume degrees.
(5) MVR is concentrated：Feed liquid is pumped into MVR inspissators, feed liquid is concentrated to Baume degrees in 28- using MVR inspissators
Between 29 ° of B é.
(6) it crystallizes：The feed liquid that will be concentrated to give, is pumped into crystallization kettle.First lead to condensed water and be cooled to 43-46 DEG C, according to every side
Magnesium acetate crystal seed is added in feed liquid 30kg.Feed liquid is waited for begin with crystal precipitation, Temperature fall is to wait for that crystal is grown up.
(7) blowing is centrifuged：After precipitating crystal, it is put into centrifuge, mother liquor is detached, obtains crude product magnesium acetate.
(8) it dries：By crude product magnesium acetate in 40-60 DEG C of drying of fluid bed.
(9) it packs：Four water acetic acid magnesium finished products will be obtained, will be packed.
Embodiment 2
(1) it synthesizes：Into the tank of sizing mixing for filling suitable quantity of water, powdery light calcined magnesia 405Kg is put into, is stirred evenly.Again will
Slurry opens stirring with glacial acetic acid 868kg input synthesis reactors.Wherein：The molar ratio of input light calcined magnesia and glacial acetic acid exists
1:2.The content of magnesia is 80%, and the content of glacial acetic acid is 98%.
(2) control reaction：Feed intake end, exothermic heat of reaction, is maintained at 80-90 DEG C of reaction temperature, keeps the temperature 2-3 hours.Control
Reaction end processed be pH value in 6-7, Baume degrees is between 15-16 ° of B é.
(3) press filtration：By the feed liquid after reaction through plate and frame filter press press filtration, filtrate is obtained.Obtained filter residue after press filtration is used
In preparing soil conditioner.
(4) scraper evaporator concentrates：Using scraper evaporator, by filtrate concentration and evaporation between 25-26 ° of B é of Baume degrees.
(5) MVR is concentrated：Feed liquid is pumped into MVR inspissators, feed liquid is concentrated to Baume degrees in 28- using MVR inspissators
Between 29 ° of B é.
(6) it crystallizes：The feed liquid being concentrated to give is pumped into crystallization kettle.First lead to condensed water and be cooled to 43-46 DEG C, according to every square stock
Magnesium acetate crystal seed is added in liquid 37Kg.Feed liquid is waited for begin with crystal precipitation, Temperature fall is to wait for that crystal is grown up.
(7) blowing is centrifuged：After precipitating crystal, it is put into centrifuge, mother liquor is detached, obtains crude product magnesium acetate.
(8) it dries：By crude product magnesium acetate in 40-60 DEG C of drying of fluid bed.
(9) it packs：Four water acetic acid magnesium finished products will be obtained, will be packed.
Embodiment 3
(1) it synthesizes：Into the tank of sizing mixing for filling suitable quantity of water, powdery light calcined magnesia 440kg is put into, is stirred evenly.Again will
Slurry opens stirring with glacial acetic acid 990kg input synthesis reactors.Wherein：The molar ratio of input light calcined magnesia and glacial acetic acid exists
1:2.1.The content of magnesia is 80%, and the content of glacial acetic acid is 98%.
(2) control reaction：Feed intake end, exothermic heat of reaction, is maintained at 80-90 DEG C of reaction temperature, keeps the temperature 2-3 hours.Control
Reaction end processed be pH value in 6-7, Baume degrees is between 15-16 ° of B é.
(3) press filtration：By the feed liquid after reaction through plate and frame filter press press filtration, filtrate is obtained.Obtained filter residue after press filtration is used
In preparing soil conditioner.
(4) scraper evaporator concentrates：Using scraper evaporator, by filtrate concentration and evaporation between 25-26 ° of B é of Baume degrees.
(5) MVR is concentrated：Feed liquid is pumped into MVR inspissators again, feed liquid is concentrated to Baume degrees in 28- using MVR inspissators
Between 29 ° of B é.
(6) it crystallizes：The feed liquid that will be concentrated to give, is pumped into crystallization kettle.First lead to condensed water and be cooled to 43-46 DEG C, according to every side
Magnesium acetate crystal seed is added in feed liquid 45Kg.Feed liquid is waited for begin with crystal precipitation, Temperature fall is to wait for that crystal is grown up.
(7) blowing is centrifuged：After precipitating crystal, it is put into centrifuge, mother liquor is detached, obtains crude product magnesium acetate.
(8) it dries：By crude product magnesium acetate in 40-60 DEG C of drying of fluid bed.
(9) it packs：The four water acetic acid magnesium finished products that will be obtained, are packed.
It indicates：In three above embodiment, glacial acetic acid calculates magnesia leaching rate according to 70%.
The technical indicator of four water acetic acid magnesium made by the present invention summarizes：See below table 1.
Table 1
| Content/% | PH value | Chlorine/ppm | Appearance | |
| Embodiment 1 | 98.5 | 8.5 | 320 | White crystal |
| Embodiment 2 | 99.1 | 8.8 | 330 | White crystal |
| Embodiment 3 | 98.9 | 9.0 | 350 | White crystal |
By data in table 1 as it can be seen that the four water acetic acid magnesium obtained using present invention process, appearance white crystal, content are existed
98% or more, chlorine is relatively stablized in 320-350ppm, pH value, maintains 7-9.Concentration is divided into two parts in present invention process,
It is energy-efficient.The invented technology is simple, and process is easy to control, and low in raw material price is easy to get, and production cost is relatively low.
Four water acetic acid magnesium made by present invention process, molecular formula C4H14O8Mg, molecular weight 214.46,72-80 DEG C of fusing point,
Density 0.8g/l.Four water acetic acid magnesium are mainly used for feed addictive, cosmetics, catalyst and the intermediate of organic synthesis；It prepares
Uranium acetate magnesium, to measure sodium；And applied to medicine, industry, deodorization, sterilization, preservative, textile dyeing, eosin dye
The fixation etc. of color, nigrosine.
Claims (8)
1. the preparation process of four water acetic acid magnesium, characterized in that
Reaction route is as follows：
Magnesia is mixed into slurry with water, then is reacted with glacial acetic acid, and feed liquid press filtration after reaction removes filter residue；It is separated by solid-liquid separation
Afterwards, filtrate crystallisation, obtains magnesium acetate crude product, and drying obtains four water acetic acid magnesium finished products；
It comprises the following steps that：
(1) it synthesizes：Into the tank of sizing mixing for filling suitable quantity of water, powdery light calcined magnesia is put into, is stirred evenly；Again by slurry and ice vinegar
Acid is put in proportion into synthesis reactor, puts into the molar ratio of light calcined magnesia and glacial acetic acid 1:1.9-2.1；
(2) it reacts：Feed intake end, exothermic heat of reaction, keeps reaction temperature and keeps the temperature；Control reaction end is pH value in 6-7, Baume
Degree is between 15-16 ° of B é；
(3) press filtration：By the feed liquid press filtration after reaction, filtrate is obtained；
(4) it concentrates：By filtrate concentration and evaporation between 25-26 ° of B é of Baume degrees；
(5) it concentrates again：Feed liquid is concentrated to Baume degrees between 28-29 ° of B é；
(6) it crystallizes：The feed liquid that will be concentrated to give, is pumped into crystallization kettle；First lead to condensed water and be cooled to 43-46 DEG C, it is brilliant that magnesium acetate is added
Kind；Feed liquid is waited for begin with crystal precipitation, Temperature fall is to wait for that crystal is grown up；
(7) blowing is centrifuged：After precipitating crystal, crystallization feed liquid is put into centrifuge, mother liquor is detached with crystal, obtains crude product vinegar
Sour magnesium；
(8) it dries：Crude product magnesium acetate is in 40-60 DEG C of drying of fluid bed；
(9) it packs：The four water acetic acid magnesium finished products that will be obtained, are packed.
2. the preparation process of four water acetic acids magnesium according to claim 1, characterized in that in the step (1), magnesia
Content is 80%, and the content of glacial acetic acid is 98%.
3. the preparation process of four water acetic acids magnesium according to claim 1, characterized in that in the step (2), keep reaction
Temperature keeps the temperature 2-3 hours at 80-90 DEG C.
4. the preparation process of four water acetic acids magnesium according to claim 1, characterized in that in the step (3), feed liquid press filtration
It is carried out in plate and frame filter press.
5. the preparation process of four water acetic acids magnesium according to claim 1 or 4, characterized in that in the step (3), feed liquid
The filter residue obtained after press filtration, is used to prepare soil conditioner.
6. the preparation process of four water acetic acids magnesium according to claim 1, characterized in that the concentration in the step (4) is
Using scraper evaporator, scraper plate concentration is carried out to filtrate.
7. the preparation process of four water acetic acids magnesium according to claim 6, characterized in that concentrating again in the step (5)
It is to utilize MVR inspissators, the feed liquid after being concentrated to scraper evaporator concentrates.
8. the preparation process of four water acetic acids magnesium according to claim 1, characterized in that in the step (6), add magnesium acetate
The quantity of crystal seed is put into according to every square stock liquid 30-45kg.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5162580A (en) * | 1988-07-12 | 1992-11-10 | Gancy Alan B | Process for the manufacture of magnesium calcium acetate |
| CN1174877A (en) * | 1997-08-18 | 1998-03-04 | 黄梅芬 | Heavy oil vanddium-inhibition agent for gas turbine or boiler in electric power plant |
-
2016
- 2016-08-18 CN CN201610694151.0A patent/CN106316829B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5162580A (en) * | 1988-07-12 | 1992-11-10 | Gancy Alan B | Process for the manufacture of magnesium calcium acetate |
| CN1174877A (en) * | 1997-08-18 | 1998-03-04 | 黄梅芬 | Heavy oil vanddium-inhibition agent for gas turbine or boiler in electric power plant |
Non-Patent Citations (2)
| Title |
|---|
| 乙酸镁的合成与应用研究;沈国良等;《化学世界》;20121231(第12期);第759—763、768、715页 * |
| 醋酸镁合成工艺的研究;沈国良等;《现代化工》;20090930;第29卷;第222—223、225页 * |
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Denomination of invention: Magnesium acetate tetrahydrate and its preparation process and Application Effective date of registration: 20211217 Granted publication date: 20180828 Pledgee: Laizhou Jinhui Financing Guarantee Co.,Ltd. Pledgor: LAIZHOU CITY LAIYU CHEMICAL Co.,Ltd. Registration number: Y2021980015244 |
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