CN111252786B - Method for removing organic matters of allyl ether byproduct salt - Google Patents
Method for removing organic matters of allyl ether byproduct salt Download PDFInfo
- Publication number
- CN111252786B CN111252786B CN202010090206.3A CN202010090206A CN111252786B CN 111252786 B CN111252786 B CN 111252786B CN 202010090206 A CN202010090206 A CN 202010090206A CN 111252786 B CN111252786 B CN 111252786B
- Authority
- CN
- China
- Prior art keywords
- salt
- solid salt
- solid
- drying
- washing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 150000003839 salts Chemical class 0.000 title claims abstract description 72
- 239000006227 byproduct Substances 0.000 title claims abstract description 26
- ATVJXMYDOSMEPO-UHFFFAOYSA-N 3-prop-2-enoxyprop-1-ene Chemical compound C=CCOCC=C ATVJXMYDOSMEPO-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000007787 solid Substances 0.000 claims description 60
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 34
- OSDWBNJEKMUWAV-UHFFFAOYSA-N Allyl chloride Chemical compound ClCC=C OSDWBNJEKMUWAV-UHFFFAOYSA-N 0.000 claims description 26
- 238000001035 drying Methods 0.000 claims description 26
- 238000005406 washing Methods 0.000 claims description 23
- 238000003786 synthesis reaction Methods 0.000 claims description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- 230000015572 biosynthetic process Effects 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 13
- 239000005416 organic matter Substances 0.000 claims description 11
- FYRWKWGEFZTOQI-UHFFFAOYSA-N 3-prop-2-enoxy-2,2-bis(prop-2-enoxymethyl)propan-1-ol Chemical compound C=CCOCC(CO)(COCC=C)COCC=C FYRWKWGEFZTOQI-UHFFFAOYSA-N 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 6
- 230000003472 neutralizing effect Effects 0.000 claims description 6
- 239000012267 brine Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims description 3
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 3
- 230000002194 synthesizing effect Effects 0.000 claims description 3
- -1 allyl ether compound Chemical class 0.000 abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 27
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 8
- 239000000706 filtrate Substances 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- JQRRFDWXQOQICD-UHFFFAOYSA-N biphenylen-1-ylboronic acid Chemical compound C12=CC=CC=C2C2=C1C=CC=C2B(O)O JQRRFDWXQOQICD-UHFFFAOYSA-N 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- 239000003444 phase transfer catalyst Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 150000005846 sugar alcohols Polymers 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000006266 etherification reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000012074 organic phase Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 238000005292 vacuum distillation Methods 0.000 description 2
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- 238000003848 UV Light-Curing Methods 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 230000035943 smell Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 229920006305 unsaturated polyester Polymers 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/14—Purification
- C01D3/18—Purification with selective solvents
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/14—Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/16—Preparation of ethers by reaction of esters of mineral or organic acids with hydroxy or O-metal groups
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a method for removing organic matters of allyl ether byproduct salt, and particularly relates to the technical field of removing organic matters of allyl ether compound byproduct salt.
Description
[ technical field ]
The invention relates to the technical field of allyl ether compounds, in particular to the technical field of organic matters for removing byproduct salts of allyl ether compounds.
[ background art ]
The allyl ether compound is generally obtained by Williamson etherification reaction of polyhydric alcohol and allyl chloride in the presence of alkali metal oxide, has the performances of isomerization, oxygen bonding, polymerization and the like due to a plurality of allyl groups and 1 hydroxyl group, is often used as a polymer monomer or a cross-linking agent for preparing an acrylic polymer type thickening agent and a super absorbent resin, is widely used for graft synthesis of unsaturated polyester, polyurethane resin, epoxy resin and UV curing resin, is increasingly applied to the field of chemical green low-carbon coatings year by year, and is an important organic compound.
The Williamson etherification reaction has the advantages of low price and easy obtainment of raw materials and relatively mild reaction, and is subjected to a great deal of targeted research by industrial workers.
Zhejiang industrial university patent CN101343213B, Zhuhai Feiyang chemical company limited patent CN101200413B, China petrochemical Qilu petrochemical company patent CN1052970C, Nanjing Weier chemical company limited patent CN100410304C propose a preparation method of pentaerythritol triallyl ether, and do not mention a treatment process of a byproduct salt.
The preparation method of trimethylolpropane diallyl ether is proposed by a patent CN110156573A of Nantong Baichuan new material Co., Ltd, a patent CN102659532B of Guangdong petrochemical industry institute and a patent CN102040486B of Shandong province chemical research institute, and a treatment process of a byproduct salt is not mentioned.
After the synthesis reaction of the allyl ether is finished, a certain amount of water is added, the mixture is cooled, stood and layered, the organic phase at the upper layer is subjected to vacuum distillation to obtain an allyl ether product, and the water at the lower layer contains a large amount of sodium chloride, excessive sodium hydroxide, unreacted polyhydric alcohol and a phase transfer catalyst, and belongs to wastewater which is difficult to treat. Therefore, the production and synthesis of allyl ether need to perfect an organic matter removal method of byproduct salt, recover raw materials, recycle and make harmless, and the method accords with the development direction of the chemical industry towards green environmental protection.
[ summary of the invention ]
In order to overcome the defects of the prior art, the invention provides a method for removing organic matters of byproduct salt of allyl ether compounds, which reduces the content of the organic matters in the byproduct salt.
A method for removing organic matters of allyl ether byproduct salt is characterized by comprising the following steps:
s1: the brine for synthesizing the allyl ether is subjected to centrifugal filtration to obtain wet solid salt, the wet solid salt is preliminarily washed by synthesis reaction generated water, and washing liquid serving as alkaline water or layered water is returned to the reaction kettle for recycling;
and S2, preliminarily washing the solid salt washed in the step S1 by using a certain amount of raw material allyl chloride, and returning the washing liquid serving as the raw material allyl chloride to the stirring kettle to participate in synthesis.
S3: drying the solid salt washed by the S2, and returning the liquid obtained after condensing the drying gas as a raw material of allyl chloride to the stirring kettle for synthesis;
s4: the dried solid salt can be further calcined to completely remove organic matters, and neutralized and washed to obtain qualified industrial salt.
Further, the allyl ether includes trimethylol diallyl ether, pentaerythritol triallyl ether, and the like.
Further, in the step S1, the content of organic matters in the solid salt is 1.5-3%, the mass ratio of the solid salt to the water generated by the synthesis reaction is 100: 30-60%, and the content of the solid salt organic matter after washing is 0.9-3%.
Further, the mass ratio of the solid salt to the allyl chloride in the step S2 is 100: 200-500, and the content of the solid salt organic matter after washing is 0.1-1%.
Further, the drying method in the step S3 is ultrasonic drying or hot nitrogen drying.
Further, the content of the solid salt organic matter in the step S3 is 0-0.3%.
Further, the industrial salt in the S4 step meets the first grade standard of the GBT5462-2016 industrial salt standard.
The beneficial effects of the invention are as follows:
according to the technical scheme provided by the invention, the raw material allyl chloride and the synthesis water are used for washing the byproduct salt solid, so that the content of organic matters in the byproduct salt is reduced, the incompletely reacted materials are recovered, and then the organic matters are completely removed by calcination after drying, and finally the industrial salt byproduct is prepared.
[ description of the drawings ]
FIG. 1 is a schematic flow chart of an embodiment of the present invention.
[ detailed description of the invention ]
The present invention may be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
A method for producing organic matters by removing allyl ether byproduct salt comprises the following steps:
s1: the brine for synthesizing the allyl ether is centrifugally filtered to obtain wet solid salt, and the wet solid salt is preliminarily washed by the water generated by the synthesis reaction. The washing liquid is used as alkaline water or cooling stratified water to return to the reaction kettle for recycling.
S2, the solid salt washed in S1 is primarily washed with a certain amount of raw allyl chloride. The washing liquid is used as raw material allyl chloride and returns to the stirring kettle to participate in synthesis.
S3: and (3) drying the washed solid salt of S2, and returning the liquid obtained by condensing the drying gas as a raw material of allyl chloride to the stirring kettle to participate in synthesis. The dried solid salt can further remove organic matters through neutralization and calcination, and is dissolved and crystallized to obtain qualified industrial salt.
The allyl ether provided by the invention comprises compounds such as trihydroxymethyl diallyl ether, pentaerythritol triallyl ether and the like. After the synthesis reaction of the allyl ether is finished, a certain amount of water is added, the mixture is cooled, kept stand and layered, the organic phase at the upper layer is subjected to vacuum distillation to obtain an allyl ether product, the water at the lower layer contains a large amount of sodium chloride, excessive sodium hydroxide, unreacted polyhydric alcohol and a phase transfer catalyst, and the content of the solid salt organic matter is measured to be 1.5-3%, and the content of the sodium hydroxide is measured to be 8-13%.
In the step S1, water is used for recovering water-soluble compounds such as sodium hydroxide, pentaerythritol, phase transfer catalyst and the like, and the recovery mechanism is as follows:
solubility of sodium chloride and sodium hydroxide in water
According to the solubility curve, the sodium hydroxide has higher solubility in water compared with sodium chloride, and the higher the water temperature is, the higher the solubility is, and the solubility can be completely dissolved only by the same amount of water at the normal temperature of 20-30 ℃.
In order to recover the sodium hydroxide as much as possible, water in excess of the sodium hydroxide is needed for washing, and the mass ratio of the solid salt to the water is preferably 100: and 40-50, measuring that the content of the washed solid salt organic matter is 0.5-1.1%, the content of the sodium hydroxide is lower than 5%, and returning the obtained washing liquid L1 to the reaction kettle to be used as cooling layering water or alkali water for synthesis.
And step S2, allyl chloride is used for recovering pentaerythritol triallyl ether, trimethylol diallyl ether and intermediates, and the recovery mechanism is as follows:
solubility curve of pentaerythritol triallyl ether and trimethylolpropane diallyl ether in allyl chloride
| Temperature of | 0 | 10 | 20 | 30 | 40 |
| Pentaerythritol triallyl ether solubility (g) | Layering | 3.8 | 4.6 | 7.4 | 11.1 |
| Solubility (g) of trimethylolpropane diallyl ether | Layering | 5.4 | 6.7 | 8.9 | 13.5 |
The solubility curve shows that allyl chloride has lower solubility to pentaerythritol triallyl ether and trimethylol diallyl ether, and the solubility is not greatly increased with higher temperature.
In order to recover allyl ether as much as possible, the raw material allyl chloride is used in a large excess, and the mass ratio of the solid salt to the allyl chloride is preferably 100: 200-500%, wherein the content of the washed solid salt organic matter is 0.1-0.3%, and the obtained washing liquid L2 is used as an allyl chloride raw material and is returned to the reaction kettle to participate in synthesis.
Allyl chloride is colorless flammable liquid and has corrosive and pungent smells, so a closed drying process for isolating oxygen needs to be selected, and ultrasonic drying or hot nitrogen drying is preferred after washing. The ultrasonic drying temperature is 90-110 ℃, the drying time is 20min, the hot nitrogen temperature is 80-95 ℃, the drying time is 45min, the drying can be completed, the organic content of the solid salt after the drying is 0-0.1%, and the liquid obtained by condensation is used as the allyl chloride raw material and returns to the reaction kettle to participate in the synthesis.
And (3) further calcining the dried solid salt in a muffle furnace at 300-400 ℃, thoroughly removing organic matters, and then neutralizing and washing to obtain the qualified industrial salt.
As shown in fig. 1, a schematic flow chart of an embodiment of the present invention is shown.
Example 1
Taking 100g of byproduct salt of pentaerythritol triallyl ether in a production device, placing the byproduct salt in a three-necked bottle with stirring, adding 30g of water at the lower layer of a water separation tank, heating to 30 ℃, stirring for 30min, and filtering to obtain a filtrate L1:47.22g, a solid S1: 82.78 g;
100g of allyl chloride was further added, and the resulting solid S1 was washed with stirring at 30 ℃ for about 30min, filtered under a closed condition, and repeated 5 times. Filtrate L2:497.15g, solid S2: 85.63 g;
starting the refrigerating fluid to-15 ℃, controlling the nitrogen flow rate to be 50ml/min, heating the three-necked bottle to 90 ℃, and collecting a condensate L3: 5.02g, cooled to give solid S4: 80.61 g;
and putting the solid S4 into a crucible, calcining for 3 hours at 300 ℃ in a muffle furnace to obtain 80.41g of solid, neutralizing and washing with 43.6ml of 10% diluted hydrochloric acid, and drying to obtain the industrial salt.
The detection results are as follows:
example 2
Taking 100g of byproduct salt of pentaerythritol triallyl ether in a production device, putting the byproduct salt into a three-necked bottle with a stirrer, adding 50g of lower-layer water in a water separation tank, heating to 30 ℃, stirring for 30min, and filtering to obtain filtrate L1:78.71g and solid S1: 71.29 g;
100g of allyl chloride was further added, and the resulting solid S1 was washed with stirring at 30 ℃ for about 30min, filtered under a closed condition, and repeated 5 times. Filtrate L2:496.85g, solid S2: 74.44 g;
starting the refrigerating fluid to-15 ℃, controlling the nitrogen flow rate to be 50ml/min, heating the three-necked bottle to 90 ℃, and collecting a condensate L3: 5.01g, cooled to give solid S4: 69.43 g;
and putting the solid S4 into a crucible, calcining for 3 hours at 300 ℃ in a muffle furnace to obtain 69.34g of solid, neutralizing and washing with 8.9ml of 10% diluted hydrochloric acid, and drying to obtain the industrial salt.
The detection results are as follows:
example 3
Taking 100g of byproduct salt of trimethylolpropane diallyl ether in a production device, putting the byproduct salt into a three-necked bottle with a stirrer, adding 50g of lower-layer water in a water separation tank, heating to 30 ℃, stirring for 30min, and filtering to obtain filtrate L1:78.92g, solid S1: 71.08 g;
100g of allyl chloride was further added, and the resulting solid S1 was washed with stirring at 30 ℃ for about 30min, filtered under a closed condition, and repeated 5 times. Filtrate L2:495.89g, solid S2: 75.19 g;
starting the refrigerating fluid to-15 ℃, controlling the nitrogen flow rate to be 50ml/min, heating the three-necked bottle to 90 ℃, and collecting a condensate L3: 5.04g, cooled to give solid S4: 70.16 g;
and putting the solid S4 into a crucible, calcining for 3 hours at 300 ℃ in a muffle furnace to obtain 69.83g of solid, neutralizing and washing with 31.7ml of 10% diluted hydrochloric acid, and drying to obtain the industrial salt.
The detection results are as follows:
example 4
Taking 100g of byproduct salt of trimethylolpropane diallyl ether in a production device, putting the byproduct salt into a three-necked bottle with stirring, adding 30g of lower-layer water in a water separation tank, heating to 30 ℃, stirring for 30min, and filtering to obtain filtrate L1:47.35g, solid S1: 82.65 g;
100g of allyl chloride was further added, and the resulting solid S1 was washed with stirring at 30 ℃ for about 30min, filtered under a closed condition, and repeated 5 times. Filtrate L2:495.89g, solid S2: 86.76 g;
starting the refrigerating fluid to-15 ℃, controlling the nitrogen flow rate to be 50ml/min, heating the three-necked bottle to 90 ℃, and collecting a condensate L3: 5.09g, cooled to give S4 as a solid: 81.67 g;
and putting the solid S4 into a crucible, calcining for 3 hours at 300 ℃ in a muffle furnace to obtain 80.9g of solid, neutralizing and washing with 66.5ml of 10% dilute hydrochloric acid, and drying to obtain the industrial salt.
The detection results are as follows:
in the above embodiment, the raw material allyl chloride and the synthesis water are used to wash the by-product salt solid, so as to reduce the content of organic matters in the by-product salt, recover the incompletely reacted materials, and then completely remove the organic matters by calcination after drying. No foreign substances are introduced into the product, the operation is simple, no secondary pollution is generated, and the utilization rate of raw materials is improved.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above embodiment, and all technical solutions belonging to the principle of the present invention belong to the protection scope of the present invention. Modifications to the disclosed embodiments will be readily apparent to those skilled in the art, and the generic principles herein may be applied to other embodiments without departing from the spirit or scope of the invention.
Claims (5)
1. A method for removing organic matters of allyl ether byproduct salt is characterized by comprising the following steps:
s1: the brine for synthesizing the allyl ether is subjected to centrifugal filtration to obtain wet solid salt, the wet solid salt is preliminarily washed by synthesis reaction generated water, and washing liquid serving as alkaline water or layered water is returned to the reaction kettle for recycling; wherein the organic matter content of the solid salt is 1.5-3%, the mass ratio of the solid salt to the water generated by the synthesis reaction is 100: 30-60%, wherein the content of the solid salt organic matter after washing is 0.9-3%;
s2, preliminarily washing the solid salt washed in the step S1 by using a certain amount of raw material allyl chloride, and returning washing liquid serving as the raw material allyl chloride to the stirring kettle to participate in synthesis; wherein the mass ratio of the solid salt to the allyl chloride is 100: 200-500%, wherein the content of the solid salt organic matter after washing is 0.1-1%;
s3: drying the solid salt washed by the S2, and returning the liquid obtained after condensing the drying gas as a raw material of allyl chloride to the stirring kettle for synthesis;
s4: and (3) further calcining the dried solid salt to completely remove organic matters, and neutralizing and washing to obtain the qualified industrial salt.
2. The method of claim 1, wherein the method comprises the steps of: the allyl ether includes trimethylol diallyl ether or pentaerythritol triallyl ether.
3. The method of claim 1, wherein the method comprises the steps of: the drying method in the step S3 is ultrasonic drying or hot nitrogen drying.
4. The method of claim 1, wherein the method comprises the steps of: and in the step S3, the content of the solid salt organic matter is 0-0.3%.
5. The method of claim 1, wherein the method comprises the steps of: the industrial salt in the step S4 meets the first-grade standard of the GBT5462-2016 industrial salt standard.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010090206.3A CN111252786B (en) | 2020-02-13 | 2020-02-13 | Method for removing organic matters of allyl ether byproduct salt |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010090206.3A CN111252786B (en) | 2020-02-13 | 2020-02-13 | Method for removing organic matters of allyl ether byproduct salt |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111252786A CN111252786A (en) | 2020-06-09 |
| CN111252786B true CN111252786B (en) | 2022-06-24 |
Family
ID=70945637
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010090206.3A Active CN111252786B (en) | 2020-02-13 | 2020-02-13 | Method for removing organic matters of allyl ether byproduct salt |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111252786B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1944502A (en) * | 2006-11-01 | 2007-04-11 | 南京威尔化工有限公司 | Synthetic method for crosslinking agent-pentaerythritol allyl ether for high molecular polymerization |
| CN104649495A (en) * | 2015-02-13 | 2015-05-27 | 江苏中丹集团股份有限公司 | Chemical industrial waste salt refining process |
| CN106745076A (en) * | 2016-11-21 | 2017-05-31 | 大唐国际化工技术研究院有限公司 | A kind of method that Industrial Wastewater Treatment is produced carnallite resource |
| CN109665660A (en) * | 2017-10-16 | 2019-04-23 | 孙汝友 | The refining methd of industrial waste salt |
| CN110105573A (en) * | 2019-05-21 | 2019-08-09 | 中国石油化工股份有限公司 | A method of reducing polyphenylene sulfide by-product salt COD |
-
2020
- 2020-02-13 CN CN202010090206.3A patent/CN111252786B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1944502A (en) * | 2006-11-01 | 2007-04-11 | 南京威尔化工有限公司 | Synthetic method for crosslinking agent-pentaerythritol allyl ether for high molecular polymerization |
| CN104649495A (en) * | 2015-02-13 | 2015-05-27 | 江苏中丹集团股份有限公司 | Chemical industrial waste salt refining process |
| CN106745076A (en) * | 2016-11-21 | 2017-05-31 | 大唐国际化工技术研究院有限公司 | A kind of method that Industrial Wastewater Treatment is produced carnallite resource |
| CN109665660A (en) * | 2017-10-16 | 2019-04-23 | 孙汝友 | The refining methd of industrial waste salt |
| CN110105573A (en) * | 2019-05-21 | 2019-08-09 | 中国石油化工股份有限公司 | A method of reducing polyphenylene sulfide by-product salt COD |
Non-Patent Citations (1)
| Title |
|---|
| 化工废盐处理与资源化技术发展现状;杨文振等;《中囯环境科学学会科学技木年会论文集》;20191231;第2190-2197页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111252786A (en) | 2020-06-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102134331A (en) | Recycling method of waste silicone rubber | |
| CN103044257A (en) | Alcoholysis method and device system for producing dioctyl terephthalate by polyester wastes | |
| CN111252786B (en) | Method for removing organic matters of allyl ether byproduct salt | |
| CN111454169B (en) | Method for recovering waste organic solvent containing N, N-dimethylacetamide | |
| CN113603584A (en) | Method for photo-thermal degradation of polyester | |
| CN117105756A (en) | Preparation method of 4-hexene-3-ketone | |
| CN101423478B (en) | A method for producing adipic acid and hexamethylenediamine by depolymerization of nylon-66 | |
| CN106902489B (en) | Method for treating CTC (CTC) distillation still residues | |
| CN111138250A (en) | A kind of purification method of chlorophenyl glycerol | |
| CN1390826A (en) | Process for depolymerizing waste polyester | |
| CN100503667C (en) | Production method of vinyl chloride-vinyl acetate-vinyl alcohol copolymer resin | |
| WO2012171446A1 (en) | Method for synthesizing tributyl citrate using compound ion liquid as catalyst | |
| CN1600690A (en) | Method for preparing bimetallic oxide and hydrotalcite with Bayer red mud as raw material | |
| CN110683988A (en) | Method for cleanly producing DTDC | |
| CN113968782A (en) | Method for removing impurities in recycled acetic acid | |
| CN1136184C (en) | Process for preparing dimethyl 2,6-naphthalene-dicarboxylate | |
| CN101735052B (en) | Method for preparing dibutyl itaconate | |
| CN106046356B (en) | The method for purifying polyether ketone ketone crude product | |
| CN205851119U (en) | A kind of polyarylate resin production centrifuge | |
| CN101735051B (en) | Method for preparing diisooctyl itaconate | |
| CN101544381B (en) | Method for producing ammonium sulphate by waste water produced in alpha naphthol production | |
| CN212174839U (en) | Device for synthesizing methallyl alcohol | |
| CN109705880A (en) | A kind of chlor-alkali salt sludge recycling technology | |
| CN1100616C (en) | Catalyst for synthesizing glycol monoether acetate and diethylene glycol monoether acetate | |
| CN112960683B (en) | Comprehensive utilization process of C5 petroleum resin polymerization liquid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20201211 Address after: 519000 first and second floors of quality inspection building, No.2, Nanhua Second Road, nanshaui Town, Gaolan Port Economic Zone, Zhuhai City, Guangdong Province Applicant after: ZHUHAI SMOOTHWAY ELECTRONIC MATERIALS Co.,Ltd. Address before: 313000 Chengnan Industrial Park, Heping Town, Changxing County, Huzhou City, Zhejiang Province Applicant before: Zhejiang Fuwei Electronic Materials Co.,Ltd. |
|
| TA01 | Transfer of patent application right | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |