CN114957334A - Post-treatment process and application of flame retardant product - Google Patents
Post-treatment process and application of flame retardant product Download PDFInfo
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- CN114957334A CN114957334A CN202110877041.9A CN202110877041A CN114957334A CN 114957334 A CN114957334 A CN 114957334A CN 202110877041 A CN202110877041 A CN 202110877041A CN 114957334 A CN114957334 A CN 114957334A
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- flame retardant
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 67
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000002002 slurry Substances 0.000 claims abstract description 27
- 239000002904 solvent Substances 0.000 claims abstract description 23
- 238000005406 washing Methods 0.000 claims abstract description 15
- 238000005119 centrifugation Methods 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract description 63
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 abstract description 32
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 abstract description 16
- 238000006243 chemical reaction Methods 0.000 abstract description 10
- 239000002360 explosive Substances 0.000 abstract description 2
- 238000007086 side reaction Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 239000011269 tar Substances 0.000 description 7
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 5
- 238000005886 esterification reaction Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- WQYSXVGEZYESBR-UHFFFAOYSA-N thiophosphoryl chloride Chemical group ClP(Cl)(Cl)=S WQYSXVGEZYESBR-UHFFFAOYSA-N 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 238000005917 acylation reaction Methods 0.000 description 3
- 239000002641 tar oil Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000032050 esterification Effects 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- 239000013557 residual solvent Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229920000297 Rayon Polymers 0.000 description 1
- 230000010933 acylation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 description 1
- 235000011180 diphosphates Nutrition 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000012946 outsourcing Methods 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 150000007970 thio esters Chemical class 0.000 description 1
- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/547—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom
- C07F9/6564—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having phosphorus atoms, with or without nitrogen, oxygen, sulfur, selenium or tellurium atoms, as ring hetero atoms
- C07F9/6571—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having phosphorus atoms, with or without nitrogen, oxygen, sulfur, selenium or tellurium atoms, as ring hetero atoms having phosphorus and oxygen atoms as the only ring hetero atoms
- C07F9/6574—Esters of oxyacids of phosphorus
- C07F9/65742—Esters of oxyacids of phosphorus non-condensed with carbocyclic rings or heterocyclic rings or ring systems
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/5398—Phosphorus bound to sulfur
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Manufacturing & Machinery (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to the technical field of flame retardants, in particular to C07F9/6574, and more particularly relates to a post-treatment process and application of a flame retardant product. A post-treatment process for a flame retardant product comprising: feeding the NLD-02 flame retardant slurry containing the solvent into a centrifuge, controlling the pressure of the centrifuge to be-10 to-20 kPa for centrifugation, removing the solvent to obtain a centrifugal product, washing with hot water, and then performing centrifugal separation again to obtain the flame retardant. The post-treatment process of the flame retardant product reduces the operation process of methanol post-treatment, reduces the consumption of methanol, reduces the consumption of rectification energy, and simultaneously reduces the generation of dangerous waste tar in a rectification tower; meanwhile, methanol is replaced by hot water washing, so that the danger of methanol which is a flammable and explosive substance in the washing process is reduced, and the intrinsic safety of the centrifugal process is improved; the reduction of methanol reduces the content of methanol in the recovered solvent pyridine, so that the side reaction is reduced, the reaction is stable and the yield is improved.
Description
Technical Field
The invention relates to the technical field of flame retardants, in particular to C07F9/6574, and more particularly relates to a post-treatment process and application of a flame retardant product.
Background
The NLD-02 flame retardant is an organic phosphorus halogen-free flame retardant and is widely applied to materials such as plastics, fibers, rubber and the like. CN201910031534 adopts trichlorophos and neopentyl glycol to carry out acylation reaction, then adds an acid-binding agent and water to carry out esterification reaction, carries out suction filtration after complete reaction, uses anhydrous methanol for recrystallization to obtain the flame retardant special for viscose fibers, has short reaction time and safe operation, adopts anhydrous methanol for recrystallization after reaction, and has the defects of tar oil formed by concentrating impurities during methanol recovery, equipment and pipelines are blocked, production control is not facilitated, tar oil filling is complicated, the field environment pollution is caused, and the tar oil needs to be subjected to outsourcing incineration treatment. CN201010276872 adopts a thioester flame retardant obtained by the reaction of cyclohexane, neopentyl glycol, trichloro-thiophosphoryl and triethylamine, and suspension is obtained after filtration and grinding, however, the suspension is not subjected to post-treatment process, and the yield is low. In addition, in the current NLD-02 flame retardant production process, because a solvent contains methanol, the reaction control uniformity is poor, the yield fluctuation is large, meanwhile, the methanol is adopted to wash impurities in the post-treatment process, and then the methanol in the washing liquid is recovered, so that the product loss along with the mother liquor is large when materials are centrifuged, and the yield is influenced.
Disclosure of Invention
In view of the problems of the prior art, the first aspect of the present invention provides a post-treatment process for a flame retardant product, comprising: feeding the NLD-02 flame retardant slurry containing the solvent into a centrifuge, controlling the pressure of the centrifuge to be-10 to-20 kPa for centrifugation, removing the solvent to obtain a centrifugal product, washing with hot water, and then performing centrifugal separation again to obtain the flame retardant.
The applicant unexpectedly finds that when the pressure of the centrifugal machine is-10 to-20 kPa, more solvent can be recovered in the later period, and the finally obtained flame retardant product has less residual solvent.
In one embodiment, the time of centrifugation is 20-40min, preferably 30 min.
The applicant has surprisingly found that when the centrifugation time is 20-40min, the final flame retardant product has a low residual solvent content.
In one embodiment, the pressure of the centrifuge is controlled to be-15 kPa.
In one embodiment, the process of feeding the NLD-02 flame retardant slurry containing a solvent to a centrifuge comprises: NLD-02 flame retardant slurry containing a solvent is fed into a centrifuge in three batches, wherein n is more than or equal to 3.
Preferably, NLD-02 flame retardant slurry containing solvent is fed into a centrifuge in three batches, and the weight ratio of the materials fed in sequence is (1.1-2): (0.8-1): (0.1-0.7), more preferably 1.5: 1: 0.5.
the applicant found in experiments that the yield of the flame retardant obtained by the conventional one-time feeding mode is reduced, and unexpectedly found that the flame retardant is fed in three batches, and the weight ratio of the sequential feeding is (1.1-2): (0.8-1): (0.1-0.7), in particular 1.5: 1: when 0.5, the yield of the obtained flame retardant is improved.
In one embodiment, the solvent-containing NLD-02 flame retardant slurry is fed into the centrifuge in three batches, the feeding time of the first batch of NLD-02 flame retardant slurry and the second batch of NLD-02 flame retardant slurry is 10-15min, and the feeding time of the third batch of NLD-02 flame retardant slurry is 1-8 min.
Preferably, the feeding time of the first batch of NLD-02 flame retardant slurry and the second batch of NLD-02 flame retardant slurry is 12min, and the feeding time of the third batch of NLD-02 flame retardant slurry is 5 min.
The applicant unexpectedly finds that the flame retardant product yield can be effectively improved when the feeding time of the first batch and the second batch is 10-15min and the feeding time of the third batch is 1-8min by controlling the speed of the flame retardant slurry entering the centrifuge.
In one embodiment, the hot water has a temperature of 35-55 ℃.
Preferably, the number of hot water washes is 2-4, preferably 3.
In one embodiment, the hot water has a temperature of 50-55 ℃ at a weight ratio of hot water to centrifuged product of less than 2 per hot water wash.
In one embodiment, the weight ratio of hot water to centrifuged product is (2-2.1): 1 hour, the hot water washing temperature is 45-55 ℃.
In one embodiment, the hot water wash temperature is 35-55 ℃ at a weight ratio of hot water to centrifuged product of greater than 2.1 per hot water wash.
The applicants have surprisingly found that with the specific hot water to centrifuge product weight ratio and hot water temperature specified herein, the tar content is reduced while the residual pyridine content is low. The applicant believes that the possible reason is that in this particular temperature range, the impurity molecules are less strongly attracted to each other and have a lower molecular mobility during washing of the centrifuged product, resulting in an increased resistance to coagulation and precipitation of the impurity molecules from each other, avoiding the formation of tars. In addition, the molecular chain of the pyrophosphate is fully stretched at the specific temperature, and the pyridine molecules are effectively removed under the action of water.
In one embodiment, the solvent is pyridine.
The preparation method of the NLD-02 flame retardant slurry containing the solvent in the present application is not particularly limited, and is obtained by performing esterification reaction on an acylation product obtained after acylation reaction of trichlorothiophosphoryl and neopentyl glycol, which is well known to those skilled in the art, in the presence of an acid-binding agent and water.
The invention also provides application of the post-treatment process of the flame retardant product in preparation of the flame retardant product.
Compared with the prior art, the invention has the following beneficial effects:
(1) when the pressure of the centrifugal machine is controlled to be-10 to-20 kPa, more solvent can be recovered in the later period, and the finally obtained flame retardant product has less solvent residue.
(2) The application adopts specific centrifugal time, so that the working efficiency is improved, and meanwhile, the finally obtained flame retardant product has less solvent residue.
(3) The application adopts specific hot water temperature and hot water content in the hot water washing process, the tar content is reduced, and the residual amount of pyridine is small.
(4) The post-treatment process of the flame retardant product reduces the operation process of methanol post-treatment, reduces the consumption of methanol, reduces the consumption of rectification energy, and simultaneously reduces the generation of dangerous waste tar in a rectification tower; meanwhile, methanol is replaced by hot water washing, so that the danger of methanol which is a flammable and explosive substance in the washing process is reduced, and the intrinsic safety of the centrifugal process is improved; the reduction of methanol reduces the content of methanol in the recovered solvent pyridine, so that the side reaction is reduced, the reaction is stable and the yield is improved.
(5) The quality index of the product obtained by the post-treatment process reaches the effect of washing by using methanol, and the oily component of the product reaches less than 0.3 wt% (index: oiliness is less than or equal to 0.7 wt%), and the product has the same washing effect with the methanol. The pyridine mother liquor obtained by the method is recycled, and the content of methanol in the recycled pyridine is less than or equal to 0.2 wt% and far lower than 0.6 wt% of the original process.
Detailed Description
The present invention is illustrated by the following specific embodiments, but is not limited to the specific examples given below.
Examples
Examples 1-15 provide post-treatment processes for a flame retardant product, respectively, as follows: feeding NLD-02 flame retardant slurry containing pyridine into a centrifuge in three batches, wherein the weight ratio of the raw materials in sequence is 1.5: 1: 0.5, feeding the first batch of NLD-02 flame retardant slurry and the second batch of NLD-02 flame retardant slurry for 12min, feeding the third batch of NLD-02 flame retardant slurry for 5min, controlling the pressure of a centrifugal machine to be-15 kPa, centrifuging for 30min, removing pyridine to obtain a centrifugal product, washing with hot water for three times, and centrifuging again to obtain the flame retardant flame.
The concrete preparation method of the pyridine-containing NLD-02 flame retardant slurry comprises the following steps:
adding neopentyl glycol into the kettle, heating in a water bath, and dropwise adding trichlorothiophosphoryl. After the dropwise addition, the reaction is carried out for 300min at the temperature of 90 ℃. After the heat preservation reaction is finished, the materials are put into an esterification kettle, the temperature of the system is reduced to 80 ℃, and a solvent pyridine is added into the esterification kettle. After the end of the dropwise addition, reaction water was added. After the addition, the temperature was kept at 50 ℃ for 540 min. And (5) after the heat preservation process is finished, adding secondary water, and finally adding a sodium hydroxide solution until the pH value is 7-8.
The weight ratio of the neopentyl glycol to the trichlorothiophosphoryl to the pyridine to the reaction water is 1:1.53:2.2: 0.08.
The amount and temperature of hot water used per hot water wash were the same, and the amount, temperature and centrifuged product used per hot water wash in examples 1-15 are shown in Table 1.
TABLE 1
Performance evaluation
The tar content: the final products from examples 1-15 were each washed with alcohol, filtered and rotary distilled to calculate the tar content.
Content of pyridine: the pyridine contents of the finally obtained products in examples 1 to 15 were respectively tested using liquid chromatography analysis.
TABLE 2
| Tar content (%) | Pyridine content (ppm) | |
| Example 1 | 0.38 | 188 |
| Example 2 | 0.35 | 165 |
| Example 3 | 0.32 | 145 |
| Example 4 | 0.28 | 115 |
| Example 5 | 0.27 | 110 |
| Example 6 | 0.35 | 155 |
| Example 7 | 0.28 | 142 |
| Example 8 | 0.26 | 112 |
| Example 9 | 0.25 | 95 |
| Example 10 | 0.24 | 90 |
| Example 11 | 0.29 | 120 |
| Example 12 | 0.27 | 112 |
| Example 13 | 0.22 | 85 |
| Example 14 | 0.21 | 82 |
| Example 15 | 0.21 | 82 |
Claims (10)
1. A post-treatment process of a flame retardant product, comprising: feeding NLD-02 flame retardant slurry containing a solvent into a centrifuge, controlling the pressure of the centrifuge to be-10 to-20 kPa for centrifugation, removing the solvent to obtain a centrifugal product, washing with hot water, and then carrying out centrifugal separation again to obtain the flame retardant slurry.
2. The post-treatment process of the flame retardant product according to claim 1, wherein the centrifugation time is 20-40 min.
3. The post-treatment process of the fire retardant product according to claim 2, wherein the process of feeding the NLD-02 fire retardant slurry containing the solvent into a centrifuge comprises: the NLD-02 flame retardant slurry containing the solvent is fed into a centrifuge in n batches, wherein n is more than or equal to 3.
4. The post-treatment process of the flame retardant product according to claim 3, wherein the NLD-02 flame retardant slurry containing the solvent is fed into a centrifuge in three batches, and the weight ratio of the fed materials is (1.1-2): (0.8-1): (0.1-0.7).
5. The post-treatment process of the flame retardant product according to claim 4, wherein the feeding time of the first batch of NLD-02 flame retardant slurry and the second batch of NLD-02 flame retardant slurry is 10-15min, and the feeding time of the third batch of LD-02 flame retardant slurry is 1-8 min.
6. Process for the post-treatment of flame-retardant products according to any of claims 1 to 5, characterized in that the temperature of the hot water is between 35 and 55 ℃.
7. The process of post-treatment of the flame retardant product of claim 6 wherein the number of hot water washes is 2-4.
8. The process for the post-treatment of a flame retardant product according to claim 7, wherein the hot water has a temperature of 50-55 ℃ at a weight ratio of hot water to centrifuged product of less than 2 per hot water wash.
9. The post-treatment process of a flame retardant product according to claim 8, wherein the weight ratio of hot water to centrifuged product is (2-2.1): 1 hour, the hot water washing temperature is 45-55 ℃.
10. Use of a post-treatment process of a flame retardant product according to any of claims 1-9 in the preparation of a flame retardant product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110877041.9A CN114957334B (en) | 2021-07-31 | 2021-07-31 | Post-treatment process and application of flame retardant product |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110877041.9A CN114957334B (en) | 2021-07-31 | 2021-07-31 | Post-treatment process and application of flame retardant product |
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| Publication Number | Publication Date |
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| CN114957334A true CN114957334A (en) | 2022-08-30 |
| CN114957334B CN114957334B (en) | 2024-03-05 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101948487A (en) * | 2010-09-09 | 2011-01-19 | 吉林市吉溧化工有限责任公司 | Method for synthesizing dithio dineopentyl phosphate fire retardant |
| CN107674096A (en) * | 2017-10-31 | 2018-02-09 | 南通江山农药化工股份有限公司 | Uninanned platform technique and its equipment of the organic disulfide for pyrophosphate fire retardant |
| CN109503662A (en) * | 2019-01-14 | 2019-03-22 | 马鞍山昂扬新材料科技有限公司 | The preparation method of viscose rayon combustion inhibitor special |
-
2021
- 2021-07-31 CN CN202110877041.9A patent/CN114957334B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101948487A (en) * | 2010-09-09 | 2011-01-19 | 吉林市吉溧化工有限责任公司 | Method for synthesizing dithio dineopentyl phosphate fire retardant |
| CN107674096A (en) * | 2017-10-31 | 2018-02-09 | 南通江山农药化工股份有限公司 | Uninanned platform technique and its equipment of the organic disulfide for pyrophosphate fire retardant |
| CN109503662A (en) * | 2019-01-14 | 2019-03-22 | 马鞍山昂扬新材料科技有限公司 | The preparation method of viscose rayon combustion inhibitor special |
Non-Patent Citations (2)
| Title |
|---|
| R. S. EDMUNDSON: "Cyclic organophosphorus compounds-III some sterically hindered pyrophosphates", TETRAHEDRON, no. 21, pages 2379 - 2387 * |
| 陈永祥等: "二硫代焦磷酸双新戊二醇酯阻燃剂的合成及表征", 化学工程师, no. 1, pages 13 - 15 * |
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