CN111995639A - Synthesis method of diethyl phosphite - Google Patents
Synthesis method of diethyl phosphite Download PDFInfo
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- CN111995639A CN111995639A CN202010943905.8A CN202010943905A CN111995639A CN 111995639 A CN111995639 A CN 111995639A CN 202010943905 A CN202010943905 A CN 202010943905A CN 111995639 A CN111995639 A CN 111995639A
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- phosphorous acid
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- diethyl phosphite
- phosphite
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- LXCYSACZTOKNNS-UHFFFAOYSA-N diethoxy(oxo)phosphanium Chemical compound CCO[P+](=O)OCC LXCYSACZTOKNNS-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000001308 synthesis method Methods 0.000 title claims description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 103
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims abstract description 75
- 238000000034 method Methods 0.000 claims abstract description 33
- 238000003756 stirring Methods 0.000 claims abstract description 24
- BDZBKCUKTQZUTL-UHFFFAOYSA-N triethyl phosphite Chemical compound CCOP(OCC)OCC BDZBKCUKTQZUTL-UHFFFAOYSA-N 0.000 claims abstract description 18
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- 238000001816 cooling Methods 0.000 claims description 7
- 230000000630 rising effect Effects 0.000 claims description 3
- 238000010923 batch production Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 abstract description 6
- 238000007086 side reaction Methods 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000003054 catalyst Substances 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 description 13
- 238000005070 sampling Methods 0.000 description 11
- 238000004321 preservation Methods 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000000543 intermediate Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 230000032050 esterification Effects 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 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 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 230000000895 acaricidal effect Effects 0.000 description 1
- 239000000642 acaricide Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003986 organophosphate insecticide Substances 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- -1 phosphate ester Chemical class 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
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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 System
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/08—Esters of oxyacids of phosphorus
- C07F9/141—Esters of phosphorous acids
- C07F9/142—Esters of phosphorous acids with hydroxyalkyl compounds without further substituents on alkyl
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
Abstract
The invention relates to a method for synthesizing diethyl phosphite, which comprises the steps of loading triethyl phosphite into a stirring reactor, adding phosphorous acid into the stirring reactor in batches under the stirring condition, wherein the times of adding phosphorous acid in batches are 4-5 times, the temperature is controlled to be less than or equal to 35 ℃ in the batch adding process of phosphorous acid, keeping the temperature of 50-60 ℃ for 30 minutes after the phosphorous acid is added, then heating at 2.5-5 ℃/h, gradually heating at 60-90 ℃ and reacting for 3-5 hours to obtain the diethyl phosphite. The method is prepared by directly reacting triethyl phosphite with phosphorous acid, does not need a solvent or a catalyst compared with the traditional process, and has mild reaction and high yield which can reach 97-99 percent; the reaction process has no side reaction, the product has good purity which can reach more than 99 percent, and the method has low cost, safety and environmental protection and is suitable for industrial production.
Description
Technical Field
The invention belongs to the field of organic synthesis of fine chemical intermediates, and particularly relates to a synthesis method of diethyl phosphite.
Background
Diethyl phosphite is an important organic synthesis intermediate, and can be used as an intermediate to prepare a flame retardant plasticizer; also can prepare organophosphorus insecticide and acaricide; can also be used for preparing phosphate ester with special requirements and preparing metal corrosion inhibitor.
So far, two methods for preparing diethyl phosphite are available, namely a direct esterification method of phosphorous acid and ethanol, and a reaction of phosphorus trichloride and absolute ethanol for synthesizing diethyl phosphite, the first method has low esterification yield, is restricted by various factors and is not suitable for industrialization, the second method needs a large amount of solvent or synthesizes a target product under an acidic condition, and the method is industrialized on a large scaleProduction, but the process is on the starting material PCl3The purity requirement is high, otherwise, potential safety hazards can be caused; in addition, side reactions occur during the production process, so that desorption and distillation are required after the synthesis is completed, the yield of the product is affected, the operation difficulty is increased, and the production cost is increased.
Disclosure of Invention
The invention aims to provide a method for synthesizing diethyl phosphite by utilizing triethyl phosphite and phosphorous acid under the conditions of low temperature and no solvent, which has the advantages of simple operation, no side reaction, low cost, safety, environmental protection and high yield.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a synthesis method of diethyl phosphite comprises the following specific steps:
putting triethyl phosphite into a stirring reactor, adding phosphorous acid into the stirring reactor in batches under the stirring condition, wherein the first feeding amount of the phosphorous acid accounts for 10% -20% of the total mass, the feeding amount of the phosphorous acid is more than or equal to that of the last feeding amount of the phosphorous acid every time, the molar ratio of the triethyl phosphite to the phosphorous acid is 2:1, the number of times of batch feeding is 4-5, the temperature is controlled to be less than or equal to 35 ℃ in the batch feeding process of the phosphorous acid, the temperature is kept for 30 minutes at 50-60 ℃ after the phosphorous acid is completely fed, then the temperature is raised at 2.5-5 ℃/h, the temperature is gradually raised at 60-90 ℃ and the reaction is carried out for 3-5 hours, and the diethyl phosphite is obtained.
In a preferred embodiment, the temperature is gradually increased and the reaction is carried out at a rate of 2.5 ℃/h.
In a preferred embodiment, the temperature is controlled between 20 ℃ and 35 ℃ during the batchwise addition of phosphorous acid, and the reaction is stirred for 15 minutes after each addition of phosphorous acid.
As a further preference, in the phosphorous acid batch process, when the reaction exotherm causes the reaction system to heat up to 32 ℃ to 33 ℃, cold water is adopted for cooling so as to control the temperature in the phosphorous acid batch feeding process.
In a preferred embodiment, the triethyl phosphite has a purity of 99.5%.
In a preferred embodiment, the concentration of the industrial phosphorous acid is 98%.
The reaction process of the invention is as follows: c6H15O3P+H3PO3→C4H11O3P。
Compared with the prior art, the invention has the following beneficial effects:
1. the method is prepared by directly reacting triethyl phosphite with phosphorous acid, does not need a solvent or a catalyst compared with the traditional process, and has mild reaction and high yield which can reach 97-99 percent;
2. the reaction is exothermic, and phosphorous acid is added in batches, so that the system is not over-temperature and the material is prevented from being flushed.
3. The method has the advantages of simple operation, no side reaction in the reaction process, good product purity, low cost, safety, environmental protection and suitability for industrial production, and the product purity can reach more than 99%.
Drawings
FIG. 1 is a gas chromatogram of diethyl phosphite synthesized in example 1 of the present invention.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
In the raw materials related to the examples of the present invention and the comparative examples, triethyl phosphite with a purity of 99.5% and industrial phosphorous acid with a mass concentration of 98% were uniformly selected.
Example 1
The specific operation process of this example is as shown in table 1, taking 41.5g triethyl phosphite into a four-neck flask at 24 ℃ and room temperature, placing the four-neck flask into a water bath, adding phosphorous acid into the four-neck flask four times under stirring, the first time phosphorous acid adding temperature is 24 ℃, the phosphorous acid adding amount is 1.025g stirring reaction for 15 minutes; because the reaction releases heat, when the first feeding and the reaction are completed, the temperature of the reaction system is raised to 27 ℃, 2.05g of phosphorous acid is added for the second time, the reaction system is stirred and reacts for 15 minutes, the temperature of the reaction system is raised to 32 ℃ because of the reaction heat release, and the temperature is reduced by cold water; when the second feeding and the reaction are completed, the temperature of the reaction system is 30 ℃, 3.075g of phosphorous acid is added for the third time, the reaction is stirred for 15 minutes, the temperature of the reaction system is increased to 33 ℃ due to the reaction heat release, and the temperature of cold water is reduced; when the third feeding and reaction is finished, the temperature of the reaction system is 29 ℃, 4.1g of phosphorous acid is fed for the fourth time, the stirring reaction is carried out for 15 minutes, and the temperature of the reaction system is controlled to be less than or equal to 35 ℃; and (3) heating the water bath kettle, controlling the temperature to be 55-60 ℃, preserving the heat for 30 minutes, then heating the water bath kettle to 72.5 ℃ at the speed of 2.5 ℃/h, and completing the reaction to obtain the product diethyl phosphite. Sampling analysis shows that the residual amount of the raw materials is 0.10%, and a gas chromatogram of diethyl phosphite is shown in figure 1.
TABLE 1
| Time of day | Temperature (. degree.C.) | Operation processes and phenomena |
| 10:00 | 24 | 41.5g of triethyl phosphite was added, and 1.025g of phosphorous acid was added thereto with stirring |
| 10:15 | 28 | 2.05g of phosphorous acid is added, heat is released to 33 ℃, and the temperature is reduced by cold water |
| 10:30 | 30 | Adding 3.075g of phosphorous acid, continuously releasing heat, and cooling with cold water |
| 10:45 | 29 | Adding 4.10g of phosphorous acid, and cooling with cold water |
| 11:00 | 35 | The water bath kettle is heated and controlled to be kept at 55-60 DEG C |
| 11:30 | 60 | The temperature rises at the speed of 2.5 ℃/h to continue the reaction |
| 16:30 | 72.5 | Sampling and analyzing, wherein the raw material is remained by 0.10 percent, and the product purity is as follows: 99.17 percent |
Example 2
The specific operation process of this example is as shown in table 2, at 24 ℃ room temperature to take triethyl phosphite 41.5g to load into four-necked flask, and put four-necked flask into water bath, under the stirring condition to add phosphorous acid into four-necked flask four times, the first phosphorous acid adding temperature is 24 ℃, phosphorous acid adding amount is 2g stirring reaction 15 minutes; because the reaction releases heat, when the first feeding and the reaction are completed, the temperature of the reaction system rises to 28 ℃, 2g of phosphorous acid is added for the second time, the reaction system is stirred and reacts for 15 minutes, the temperature of the reaction system rises to 33 ℃ because of the reaction heat release, and the temperature of cold water is reduced; when the second feeding and the reaction are completed, the temperature of the reaction system is 30 ℃, 2g of phosphorous acid is fed for the third time, the reaction is stirred for 15 minutes, the temperature of the reaction system is raised to 33 ℃ due to the heat released by the reaction, and the temperature of the reaction system is reduced by cold water; when the third feeding and reaction is completed, the temperature of the reaction system is 29 ℃, 2g of phosphorous acid is fed for the fourth time, the reaction is stirred for 15 minutes, the temperature of the reaction system is raised to 33 ℃ due to the reaction heat release, and the temperature of the reaction system is reduced by cold water; and when the fourth feeding and reaction is finished, the temperature of the reaction system is 29 ℃, 2g of phosphorous acid is fed for the fifth time, the heat preservation and stirring are carried out for 15 minutes, the water bath kettle is heated to control the temperature to be 55-60 ℃ and is kept for 30 minutes, then the temperature is raised to 72.5 ℃ at the speed of 2.5 ℃/h, and the reaction is finished, so that the product diethyl phosphite is obtained. Sampling and analyzing, and the purity of the product is 98.06%.
TABLE 2
| Time of day | Temperature (. degree.C.) | Operation processes and phenomena |
| 10:00 | 24 | 41.5g of triethyl phosphite was added, and 2g of phosphorous acid was added thereto with stirring |
| 10:15 | 28 | 2g of phosphorous acid is added, the heat is released to 33 ℃, and the temperature is reduced by cold water |
| 10:30 | 30 | 2g of phosphorous acid is added, heat release is continued, and the temperature is reduced by cold water |
| 10:45 | 29 | 2g of phosphorous acid is added, and the temperature is reduced by cold water |
| 11:00 | 29 | 2.25g of phosphorous acid is added, the temperature is slightly released, and the temperature can be reduced without cold water and is kept |
| 11:30 | 35 | The water bath kettle is heated and controlled to be kept at 55-60 DEG C |
| 12:00 | 60 | Sampling and analyzing, wherein the raw material is remained by 2.59 percent, and the product purity is as follows: 95.97%, heating |
| 14:00 | 65 | Sampling and analyzing, wherein the raw material is remained by 1.43 percent, and the product purity is as follows: 96.82%, heating |
| 16:00 | 70 | Sampling and analyzing, wherein the raw material is remained by 0.88%, and the product purity is as follows: 97.37% of heat rising |
| 17:00 | 72.5 | Sampling and analyzing, wherein the raw material is remained by 0.30 percent, and the product purity is as follows: 98.06 percent |
As can be seen from Table 2, after the temperature is maintained at 55-60 ℃, the reaction time is prolonged along with the rise of the temperature, the raw materials react more fully, when the temperature rises to 72.5 ℃, the raw materials react basically, the temperature continues to rise for 90 ℃, and the purity of the product is basically unchanged, so that the reaction can be completed by gradually rising the temperature at 60-72.5 ℃ and reacting for 5 hours, the purity of the product can reach 98.06%, the purity of the product is higher, further purification is not needed, and the operation is simple.
Example 3
The specific operation process of this example is as shown in table 3, taking 41.5g triethyl phosphite at 24 ℃ room temperature and placing into a four-neck flask, placing the four-neck flask into a water bath, adding phosphorous acid into the four-neck flask four times under stirring, the first time phosphorous acid adding temperature is 24 ℃, the phosphorous acid adding amount is 2g stirring reaction for 15 minutes; because the reaction releases heat, when the first feeding and the reaction are completed, the temperature of the reaction system rises to 28 ℃, 2g of phosphorous acid is added for the second time, the reaction system is stirred and reacts for 15 minutes, the temperature of the reaction system rises to 33 ℃ because of the reaction heat release, and the temperature of cold water is reduced; when the second feeding and the reaction are completed, the temperature of the reaction system is 30 ℃, 2g of phosphorous acid is fed for the third time, the reaction is stirred for 15 minutes, the temperature of the reaction system is raised to 33 ℃ due to the heat released by the reaction, and the temperature of the reaction system is reduced by cold water; when the third feeding and reaction is completed, the temperature of the reaction system is 29 ℃, 2g of phosphorous acid is fed for the fourth time, the reaction is stirred for 15 minutes, the temperature of the reaction system is raised to 33 ℃ due to the reaction heat release, and the temperature of the reaction system is reduced by cold water; and when the fourth feeding and reaction is finished, the temperature of the reaction system is 29 ℃, 2g of phosphorous acid is fed for the fifth time, the heat preservation and stirring are carried out for 15 minutes, the water bath kettle is heated to control the temperature to be 55-60 ℃ and is kept for 30 minutes, then the temperature is raised to 90 ℃ at the speed of 5 ℃/h, and the reaction is finished, so that the product diethyl phosphite is obtained. The product purity was 97.91% by sampling.
Comparative example 1
The specific operation process of this example is as shown in table 3, taking 41.5g triethyl phosphite at 24 ℃ room temperature and placing into a four-neck flask, placing the four-neck flask into a water bath, adding phosphorous acid into the four-neck flask four times under stirring, the first time phosphorous acid adding temperature is 24 ℃, the phosphorous acid adding amount is 2g stirring reaction for 15 minutes; because the reaction releases heat, when the first feeding and the reaction are completed, the temperature of the reaction system rises to 28 ℃, 2g of phosphorous acid is added for the second time, the reaction system is stirred and reacts for 15 minutes, the temperature of the reaction system rises to 33 ℃ because of the reaction heat release, and the temperature of cold water is reduced; when the second feeding and the reaction are completed, the temperature of the reaction system is 30 ℃, 2g of phosphorous acid is fed for the third time, the reaction is stirred for 15 minutes, the temperature of the reaction system is raised to 33 ℃ due to the heat released by the reaction, and the temperature of the reaction system is reduced by cold water; when the third feeding and reaction is completed, the temperature of the reaction system is 29 ℃, 2g of phosphorous acid is fed for the fourth time, the reaction is stirred for 15 minutes, the temperature of the reaction system is raised to 33 ℃ due to the reaction heat release, and the temperature of the reaction system is reduced by cold water; and when the fourth feeding and reaction is finished, the temperature of the reaction system is 29 ℃, 2g of phosphorous acid is fed for the fifth time, the heat preservation and stirring are carried out for 15 minutes, the water bath kettle is heated to control the temperature to be 55-60 ℃, the heat preservation is carried out for 30 minutes, then the temperature is increased to 80 ℃ at the speed of 5 ℃/h, and the reaction is finished, so that the product diethyl phosphite is obtained. Sampling and analyzing, and the purity of the product is 96.97%. As is clear from comparison with example 3, the remaining amount of the raw materials in comparative example 1 was 1.39%, and a part of the raw materials were not completely reacted, and the reaction was continued by raising the temperature, whereby the purity and yield of the product could be improved.
TABLE 3
| Time of day | Temperature (. degree.C.) | Operation processes and phenomena |
| 10:00 | 24 | 41.5g of triethyl phosphite was added, and 2g of phosphorous acid was added thereto with stirring |
| 10:15 | 28 | Adding 2g of phosphorous acid, releasing heat to 33 ℃, and cooling with cold water |
| 10:30 | 30 | Adding 2g of phosphorous acid, continuously releasing heat, and cooling with cold water |
| 10:45 | 29 | Adding 2g of phosphorous acid, and cooling with cold water |
| 11:00 | 29 | 2.25g of phosphorous acid is added, the temperature is slightly released, and the temperature can be reduced without cold water and is kept |
| 11:30 | 35 | The water bath kettle is heated and controlled to be kept at 55-60 DEG C |
| 12:00 | 60 | Temperature rise is started |
| 14:00 | 80 | Sampling and analyzing, wherein the raw material is remained by 1.39%, and the product purity is as follows: 96.97 percent |
| 15:00 | 90 | Sampling and analyzing, wherein the raw material is remained by 0.39%, and the product purity is as follows: 97.91 percent |
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. A synthesis method of diethyl phosphite is characterized in that: the method comprises the following specific steps:
putting triethyl phosphite into a stirring reactor, adding phosphorous acid into the stirring reactor in batches under the stirring condition, wherein the first feeding amount of the phosphorous acid accounts for 10% -20% of the total mass, the feeding amount of the phosphorous acid is more than or equal to that of the last feeding amount of the phosphorous acid every time, the molar ratio of the triethyl phosphite to the phosphorous acid is 2:1, the number of times of batch feeding is 4-5, the temperature is controlled to be less than or equal to 35 ℃ in the batch feeding process of the phosphorous acid, the temperature is kept for 30 minutes at 50-60 ℃ after the phosphorous acid is completely fed, then the temperature is raised at 2.5-5 ℃/h, the temperature is gradually raised at 60-90 ℃ and the reaction is carried out for 3-5 hours, and the diethyl phosphite is obtained.
2. The method for synthesizing diethyl phosphite of claim 1, wherein: the temperature is gradually increased and the reaction is carried out, wherein the temperature rising speed is 2.5 ℃/h.
3. The method for synthesizing diethyl phosphite of claim 1, wherein: in the process of adding the phosphorous acid in batches, the temperature is controlled to be between 20 and 35 ℃, and the phosphorous acid is added each time and then stirred for reaction for 15 minutes.
4. The method for synthesizing diethyl phosphite of claim 3, wherein: in the phosphorous acid batch process, when the reaction heat release enables the temperature of the reaction system to rise to 32-33 ℃, cold water is adopted for cooling so as to control the temperature in the phosphorous acid batch adding process.
5. The method for synthesizing diethyl phosphite of claim 1, wherein: the purity of the triethyl phosphite is 99.5%.
6. The method for synthesizing diethyl phosphite of claim 1, wherein: the concentration of the industrial phosphorous acid is 98%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116396324A (en) * | 2023-03-17 | 2023-07-07 | 南雄志一精细化工有限公司 | Preparation method of light-colored diphenyl phosphite |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4342709A (en) * | 1980-12-08 | 1982-08-03 | Stauffer Chemical Company | Process for producing diethyl phosphite |
| CN102827202A (en) * | 2012-09-18 | 2012-12-19 | 湖北三才堂化工科技有限公司 | Technology for preparing diethyl phosphite by by-product of triethyl phosphite |
-
2020
- 2020-09-10 CN CN202010943905.8A patent/CN111995639A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4342709A (en) * | 1980-12-08 | 1982-08-03 | Stauffer Chemical Company | Process for producing diethyl phosphite |
| CN102827202A (en) * | 2012-09-18 | 2012-12-19 | 湖北三才堂化工科技有限公司 | Technology for preparing diethyl phosphite by by-product of triethyl phosphite |
Non-Patent Citations (1)
| Title |
|---|
| 陈云建 等: "微反应制备亚磷酸二乙酯的工艺研究", 《云南化工》, vol. 44, no. 8, 31 August 2017 (2017-08-31), pages 25 - 28 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116396324A (en) * | 2023-03-17 | 2023-07-07 | 南雄志一精细化工有限公司 | Preparation method of light-colored diphenyl phosphite |
| CN116396324B (en) * | 2023-03-17 | 2024-01-02 | 南雄志一精细化工有限公司 | Preparation method of light-colored diphenyl phosphite |
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