CN115611795A - Synthesis method of diisobutyryl peroxide - Google Patents
Synthesis method of diisobutyryl peroxide Download PDFInfo
- Publication number
- CN115611795A CN115611795A CN202211024529.8A CN202211024529A CN115611795A CN 115611795 A CN115611795 A CN 115611795A CN 202211024529 A CN202211024529 A CN 202211024529A CN 115611795 A CN115611795 A CN 115611795A
- Authority
- CN
- China
- Prior art keywords
- peroxide
- solution
- reaction
- synthesis method
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C407/00—Preparation of peroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F10/00—Homopolymers and copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F10/02—Ethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F14/00—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
- C08F14/02—Monomers containing chlorine
- C08F14/04—Monomers containing two carbon atoms
- C08F14/06—Vinyl chloride
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F18/00—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, of carbonic acid or of a haloformic acid
- C08F18/02—Esters of monocarboxylic acids
- C08F18/04—Vinyl esters
- C08F18/08—Vinyl acetate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F20/00—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F20/02—Monocarboxylic acids having less than ten carbon atoms, Derivatives thereof
- C08F20/10—Esters
- C08F20/12—Esters of monohydric alcohols or phenols
- C08F20/14—Methyl esters, e.g. methyl (meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/28—Oxygen or compounds releasing free oxygen
- C08F4/32—Organic compounds
- C08F4/34—Per-compounds with one peroxy-radical
Abstract
The invention provides a synthesis method of diisobutyronitrile peroxide, which relates to the technical field of initiator production and comprises the following steps: (1) Uniformly mixing the alkaline solution and hydrogen peroxide, and reacting to obtain a mixed solution 1; (2) uniformly mixing isobutyryl chloride with the mixed solution 1, and reacting; (3) And after the reaction is finished, carrying out liquid separation, washing and liquid separation on the reaction liquid to obtain the diisobutyronitrile peroxide. The method has high reaction rate, can reduce the occurrence of side reactions and improve the yield of the diisobutyronitrile peroxide, and the prepared diisobutyronitrile peroxide as an initiator can be applied to the preparation of polyethylene resin, polyvinyl chloride resin, polyvinyl acetate resin and organic glass.
Description
Technical Field
The invention belongs to the technical field of initiator production, and particularly relates to a synthesis method of diisobutyryl peroxide.
Background
Diisobutyronitrile peroxide (IBP) is a diacyl peroxide initiator, has the characteristics of high oxygen content, good low-temperature activity and the like, and is mainly used as an initiator for synthesizing high-molecular polymers in the industries of polyethylene, vinyl chloride, vinyl acetate polymerization, organic glass and the like. The peroxide is also a D-type liquid organic peroxide, has poor thermal stability, can be decomposed at 0 ℃ in a self-accelerating manner, and is easy to explode. In addition, isobutyryl chloride, a raw material for synthesizing IBP, is easy to hydrolyze, and is hydrolyzed more quickly under an alkaline condition, so that the IBP yield is not improved.
Through research, the diisobutyryl peroxide initiator has short half-life: 0.1h:57 ℃,1h:39 ℃,10h:23 ℃; belongs to an ultra-efficient initiator, and is used in a small amount as an initiator in continuous polymerization reaction of polyethylene, vinyl chloride, vinyl acetate and the like, and no residue is left in resin. However, few reports on the synthesis method of bis-isobutyryl peroxide exist, and few research works on bis-isobutyryl peroxide have been reported.
The Chinese patent with publication number CN111072542A discloses a method for continuously producing diisobutyl peroxide by multipoint feeding and reinforced mixing, which comprises the following steps: (1) Continuously feeding aqueous hydrogen peroxide and an aqueous alkali solution stream 1 into a first flow reactor for salt forming reaction; (2) Carrying out IBP generation reaction on the reaction liquid obtained in the step (1) and isobutyryl chloride solution stream 1 which is continuously added in a second flow reactor; (3) Enabling the reaction liquid obtained in the step (2) and an aqueous alkali stream 2 which is continuously added to enter a third flow reactor for salt forming reaction; (4) And (4) carrying out the reaction of generating IBP on the reaction liquid obtained in the step (3) and isobutyryl chloride solution stream 2 which is continuously added in a fourth flow reactor. The method reduces the occurrence of side reactions such as acyl chloride hydrolysis and the like, improves the yield of IBP, and timely removes reaction heat, so that the whole reaction is carried out under safe and environment-friendly continuous conditions. However, the microchannel continuous flow technology has small reaction amount, large equipment investment and limited productivity.
The research and development work of the bis-isobutyryl peroxide is carried out in the literature of 'Synthesis of bis-isobutyryl peroxide' (Qin Rong Guang, wang Yun Fang, et al, academic university of northwest (Nature science edition), 1982 (02): 77-82.), isobutyric acid is used as a raw material, and the bis-isobutyryl peroxide is prepared by two steps of reaction of acyl chlorination and peroxidation, wherein in the step of synthesizing the bis-isobutyryl peroxide, isobutyryl chloride is dropwise added into hydrogen peroxide, naOH and white oil are added under the condition of cooling, and isobutyryl chloride is dropwise added within 1 hour, and the water phase is removed, so that the bis-isobutyryl peroxide is obtained, and the yield of the product of the method is 70.7 percent, and the purity is 51.0 percent.
The side chain of the diisobutyryl peroxide is short, isobutyryl chloride is easy to hydrolyze, and the isobutyryl chloride is quicker under the alkaline condition, which is not beneficial to the characteristic of improving the yield of IBP. The problem to be solved urgently by the personnel in the technical field of initiator production at present is to improve the yield of IBP.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a synthesis method of diisobutyryl peroxide, aiming at overcoming the defects in the previous research, and the synthesis method of diisobutyryl peroxide is provided, and has the advantages of high reaction rate, capability of reducing the occurrence of side reactions and improvement on the yield of diisobutyryl peroxide. The prepared diisobutyryl peroxide can be used as an initiator to be applied to preparation of polyethylene resin, polyvinyl chloride resin, polyvinyl acetate resin and organic glass.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
firstly, the invention provides a method for synthesizing diisobutyryl peroxide, which comprises the following steps:
(1) Uniformly mixing the alkaline solution and hydrogen peroxide, and reacting to obtain a mixed solution 1;
(2) Uniformly mixing isobutyryl chloride with the mixed solution 1, and reacting;
(3) And after the reaction is finished, carrying out liquid separation, washing and liquid separation on the reaction liquid to obtain the diisobutyronitrile peroxide.
Preferably, in the step (1), the alkaline solution is at least one selected from a sodium hydroxide solution and a potassium hydroxide solution.
Further preferably, the concentration of the sodium hydroxide solution is 25-40%, and the concentration of the potassium hydroxide solution is 80-95%.
Still more preferably, the concentration of the sodium hydroxide solution is 30-35% and the concentration of the potassium hydroxide solution is 85-90%.
Still more preferably, the concentration of the sodium hydroxide solution is 32% and the concentration of the potassium hydroxide solution is 90%.
Preferably, in the step (1), the solvent of the alkaline solution is desalted water, and the conductivity is 0-5us/cm.
Preferably, in the step (1), the concentration of the hydrogen peroxide is 20-50%.
Further preferably, the concentration of the hydrogen peroxide is 25-35%.
More preferably, the concentration of the hydrogen peroxide is 27.5%.
Preferably, in the step (1), the reaction time is 20-60min, and the reaction temperature is-5-5 ℃.
Further preferably, the reaction time of the reaction is 30-40min, and the reaction temperature is 0-5 ℃.
Preferably, in the step (2), the isobutyryl chloride is uniformly mixed with the mixed solution 1, specifically: isobutyryl chloride is dripped into the mixed solution 1 within 1.5 to 3.5 hours, and the dripping temperature is between 5 ℃ below zero and 5 ℃.
Further preferably, the isobutyryl chloride is uniformly mixed with the mixed solution 1, specifically: isobutyryl chloride is dripped into the mixed solution 1 within 2-3h, and the dripping temperature is-5-0 ℃.
Preferably, in the step (2), the reaction time is 20-60min, and the temperature is-5-0 ℃.
Further preferably, the reaction time is 30-60min.
Preferably, in the step (2), the mass ratio of the isobutyryl chloride to the alkaline solution on a dry basis is 1.
Further preferably, in the step (2), the mass ratio of the isobutyryl chloride to the alkaline solution on a dry basis is 1.5-1.5, and the mass ratio of the isobutyryl chloride to the hydrogen peroxide is 1.2-1.5.
Preferably, in the step (3), the separating, washing and separating specifically include: standing the reaction solution at-10 deg.C-0 deg.C for 0-60min, separating water layer to obtain mother liquor, washing the mother liquor with washing liquid to pH8-10, standing at-10 deg.C-0 deg.C to remove water layer, and repeating for 2-4 times to obtain diisobutyryl peroxide.
Further preferably, the washing solution is at least one selected from sodium bicarbonate and sodium carbonate.
Preferably, in step (3), the temperature of the washing is from-10 ℃ to-5 ℃.
The present invention also provides diisobutyryl peroxide obtained by the above synthesis method.
Finally, the invention provides the application of the diisobutyronitrile peroxide in preparing polyethylene resin, polyvinyl chloride resin, polyvinyl acetate resin and organic glass.
Compared with the prior art, the invention has the following beneficial effects:
(1) The diisobutyronitrile peroxide prepared by the synthesis method provided by the invention is rapidly initiated in PVC and other polymerization reactions, belongs to a high-efficiency initiator, has the characteristics of continuous feeding of the initiator, small using amount and small product residual quantity, and can produce products with stable quality. Compared with the traditional initiator, the initiator has the advantages of rapid initiation and uniform heat release in the reaction process, and the obtained PVC resin conforms to the range of superior products;
(2) The synthesis method adopts alkaline substances to carry out catalytic reaction, reduces the cost of sodium hydroxide, has higher catalytic activity of potassium hydroxide, accelerates the reaction rate of isobutyryl chloride under alkaline conditions, reduces the hydrolysis of isobutyryl peroxide, and further improves the reaction yield, and the yield of the diisobutyryl peroxide under the conditions can reach more than 94 percent;
(3) According to the properties of the raw materials, the optimal reaction time and reaction temperature are determined, the decomposition of the synthesized isobutyryl peroxide in the reaction process is inhibited, and the yield is ensured;
(4) Washing is carried out by adopting a washing solution to remove chloride ions generated by the reaction, so that the problems of resin fisheyes, overproof screen residue indexes and the like in the polymerization process are effectively avoided; the pH of the initiator after washing is between 8 and 10, which is the same as the pH of the polymerization system.
Detailed Description
The following non-limiting examples are presented to enable those of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way. The following is merely an illustrative description of the scope of the invention claimed herein, and those skilled in the art can make various changes and modifications to the invention of the present application based on the disclosure, which should also fall within the scope of the invention claimed herein.
The present invention will be further described below by way of specific examples. The various chemicals used in the examples of the present invention were obtained by conventional commercial routes unless otherwise specified.
The yield calculation method comprises the following steps:
w1: the weight of the synthesized product; w2: theoretical weight of synthesized product.
The purity determination method comprises the following steps:
the polymerization is carried out by referring to the group standard 403.31-0092-vinyl chloride and detecting by an initiator, namely bis (2-ethylhexyl) peroxydicarbonate (EHP) method, wherein the solid content detection interval, namely the molecular weight of the EHP is replaced by 174.19;
dissolving a sample in a mixture of isopropanol, glacial acetic acid and water, adding a potassium iodide solution, oxidizing potassium iodide by organic peroxide under an acidic condition to quantitatively generate iodine, reacting the iodine with a quantitative sodium thiosulfate standard solution to be reduced again, and calculating the amount of the organic peroxide according to the amount of the consumed sodium thiosulfate standard solution;
and (3) specific detection of purity: in a dry 250mL iodometric vial, 30mL isopropanol and 2mL glacial acetic acid were added to the dosing cylinder, stoppered and shaken well. 0.5 g. + -. 0.02g of sample (accurate to 0.0001 g) was weighed into an iodometric vial and shaken well. 4mL of potassium iodide solution was added to the iodometry vial, the stopple was immediately added, the iodometry vial was slowly rotated, the iodometry vial was water-sealed, and the mixture was left standing for 15min in the dark. Adding 50mL of water, titrating to light yellow by using a sodium thiosulfate standard titration solution, adding 2mL of starch indicator, titrating by using the sodium thiosulfate standard titration solution until blue-black disappears, and recording the volume of the sodium thiosulfate standard titration solution consumed by titration. Simultaneously, performing a blank test;
diisobutyryl peroxide content (purity) w = (v-v) 0 )×C Na2S2O3 ×0.0871÷m Sample(s) (ii) a Wherein, v-v 0 Volume of sodium thiosulfate standard titration solution consumed for titration, mL, C Na2S2O3 Concentration of sodium thiosulfate Standard solution, g/mL, m Sample (I) Is the mass of the sample, g.
And (3) detecting chloride ions:
5 g. + -. 0.2g of sample (accurate to 0.0001 g) was weighed into a dry 250mL Erlenmeyer flask, 20mL of absolute ethanol was added, and the Erlenmeyer flask was shaken to completely dissolve the sample. Adding 20mL of sodium hydroxide solution, shaking gently for 2min, standing for 30min (shaking 2 times), adding 20mL of nitric acid solution, and cooling to room temperature. Transferring 10mL of silver nitrate standard solution by a pipette, adding 2mL of ferric ammonium sulfate indicating solution, and titrating by using potassium thiocyanate standard titration solution (injection: when the end point is approached, a conical flask needs to be shaken violently to adsorb Ag + Precipitation) until a pale brick red color appeared for 30 s. Simultaneously, performing a blank test;
content of chloride ion: w = (v) 0 -v)×C KSCN ×0.3546÷m Sample (I) ；v-v 0 Volume of potassium thiocyanate Standard titration solution consumed for titration, mL, C KSCN The concentration of standard potassium thiocyanate solution is g/mL, m Sample (I) Is the mass of the sample, g.
In the following examples, the isobutyryl chloride was obtained from Tianjin GmbH.
Example 1
(1) Mixing 62.5g of 32% sodium hydroxide solution with 62.5g of 90% potassium hydroxide solution, stirring for 20min, and cooling to 0 ℃ to obtain alkaline solution; stirring and mixing the alkaline solution and 140g of 27.5% hydrogen peroxide solution, stirring and reacting for 30min, and cooling to 0 ℃ to obtain a mixed solution;
(2) Slowly and uniformly dripping 107g of isobutyryl chloride into the mixed solution obtained in the step (1), stirring while dripping, controlling the temperature at 0 ℃, and finishing the addition of the isobutyryl chloride within 120 min; after the isobutyryl chloride is dripped, stirring and reacting for 30min at the temperature of 0 ℃;
(3) And after the reaction is finished, stopping stirring, cooling to-5 ℃, standing for 20min for layering, removing a water layer, washing the mother liquor twice by using 5% sodium bicarbonate, washing to pH9, cooling to-5 ℃ again, standing for 20min for layering, and removing the water layer to obtain the diisobutyronitrile peroxide.
Example 2
Unlike example 1, in step (1), 125g of 32% sodium hydroxide solution, 30g of 90% potassium hydroxide;
the rest conditions and steps are the same, and diisobutyryl peroxide is obtained.
Example 3
Different from the embodiment 1, in the step (1), the concentration of hydrogen peroxide is 50%, and the stirring reaction is carried out for 60min;
the other conditions and steps are the same, and diisobutyryl peroxide is obtained.
Example 4
Different from the embodiment 1, in the step (3), after the isobutyryl chloride is dripped, the mixture is stirred and reacts for 60min at the temperature of 0 ℃;
the rest conditions and steps are the same, and diisobutyryl peroxide is obtained.
Example 5
Unlike example 1, in step (1), 390g of the alkaline solution was replaced with 390g of 32% sodium hydroxide solution without adding potassium hydroxide;
the remaining conditions and procedures were the same. The product diisobutyryl peroxide is obtained.
Example 6
Unlike example 1, in step (1), the amount of the alkaline solution was 140g instead of 90% potassium hydroxide solution, and sodium hydroxide was not added;
the remaining conditions and procedures were the same. The product diisobutyryl peroxide is obtained.
Comparative example 1
Different from the embodiment 1, in the step (2), 107g of isobutyryl chloride is slowly dripped into the mixed solution obtained in the step (1) at a constant speed, stirring is carried out while dripping, the temperature is controlled at 10 ℃, and the isobutyryl chloride is completely added within 120 min; after the isobutyryl chloride is dripped, stirring and reacting for 30min at the temperature of 10 ℃;
the remaining conditions and procedures were the same. The product diisobutyryl peroxide is obtained.
Comparative example 2
In contrast to example 1, in step (3), isobutyryl chloride was added over 60min;
the remaining conditions and procedures were the same. The product diisobutyryl peroxide is obtained.
Comparative example 3
In contrast to example 1, in step (3), isobutyryl chloride was added over 240 min;
the remaining conditions and procedures were the same. The product diisobutyryl peroxide is obtained.
Comparative example 4
Unlike example 1, in step (4), there is no washing process after removing the aqueous layer by standing.
The remaining conditions and procedures were the same. The product diisobutyryl peroxide is obtained.
Comparative example 5
Unlike example 1, the temperatures in both step (2) and step (3) were replaced with-10 ℃;
the rest conditions and steps are the same, and the product of diisobutyryl peroxide is obtained.
Comparative example 6
Different from the embodiment 1, the isobutyryl chloride in the step (3) is replaced by a 30% isobutyryl chloride solution prepared by isododecane;
the remaining conditions and procedures were the same. The product diisobutyryl peroxide is obtained.
The purity, yield and chloride ion content of the diisobutyryl peroxide obtained in examples 1 to 6 and comparative examples 1 to 6 are shown in Table 1.
TABLE 1
As can be seen from Table 1, the products of examples 1-6 have relatively high yields and purities, the yield being greater than 95%, and the chloride ion being about 100 ppm. The yield is increased along with the increase of the proportion of the potassium hydroxide and the hydrogen peroxide; in example 5, potassium hydroxide solid is not added, potassium ion catalysis is not performed, the reaction rate is slow, isobutyryl chloride is hydrolyzed in the reaction process, so that the solid content and the yield are reduced, and unreacted isobutyryl chloride remains in the oil phase, so that the chloride ion content is increased; comparative example 1 the reaction temperature was controlled at 10 c resulting in a yield reduction to 67.32% due to the temperature sensitivity of the product diisobutyryl peroxide, which resulted in partial product decomposition at 10 c. The isobutyryl chloride of the comparative example 2 is added in 60min, the yield is 75.34%, the dropping speed is high, so that the isobutyryl chloride can not excessively react with sodium peroxide and potassium peroxide, the isobutyryl chloride is hydrolyzed, and the yield is influenced; the isobutyryl chloride of the comparative example 3 is added up at 240min, the yield is 90.24%, and is slightly reduced compared with the example, which shows that the reaction reaches the end point, and the product of the diisobutyryl peroxide is decomposed after the prolonged time; comparative example 4 has no washing step, which results in 2189ppm of oil phase chloride ions after reaction and over-high chlorine of chloride ions, which causes the problem of overproof indexes such as resin fisheyes, surplus and the like in the downstream polymerization process; comparative example 5 the reaction temperature is-10 ℃, the yield is 88.24%, the temperature is too low, the reaction rate is slow, and the industrial energy consumption is high; in comparative example 6, isododecane is used as a solvent to dilute the concentration of isobutyryl chloride, the reaction process is slow, but the reaction end point can be reached in the reaction process, the solvent isododecane easily wraps a water phase, the content of chloride ions is increased, the solvent isododecane is flammable, diisobutyryl peroxide is easily decomposed, a large amount of heat is released in the reaction process, and safety accidents such as deflagration and the like can be caused.
Finally, it should be noted that the above-mentioned contents are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, and that the simple modifications or equivalent substitutions of the technical solutions of the present invention by those of ordinary skill in the art can be made without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The invention provides a method for synthesizing diisobutyl peroxide, which is characterized by comprising the following steps:
(1) Uniformly mixing the alkaline solution and hydrogen peroxide, and reacting to obtain a mixed solution 1;
(2) Uniformly mixing isobutyryl chloride with the mixed solution 1, and reacting;
(3) And after the reaction is finished, carrying out liquid separation, washing and liquid separation on the reaction liquid to obtain the diisobutyronitrile peroxide.
2. The synthesis method according to claim 1, wherein in the step (1), the alkaline solution is at least one selected from a sodium hydroxide solution and a potassium hydroxide solution, the concentration of the alkaline solution is 25-40%, and the mass fraction of potassium hydroxide is 80-95%.
3. The synthesis method according to claim 1, wherein in the step (1), the concentration of the hydrogen peroxide is 20-50%.
4. The synthesis method according to claim 1, wherein in the step (1), the reaction time is 20-60min, and the reaction temperature is-5-5 ℃.
5. The synthesis method according to claim 1, wherein in the step (2), the isobutyryl chloride is uniformly mixed with the mixed solution 1, and specifically comprises the following steps: isobutyryl chloride is dripped into the mixed solution 1 within 1.5-3.5h, and the dripping temperature is-5-5 ℃.
6. The synthesis method according to claim 1, wherein in the step (2), the reaction time is 20-60min, and the temperature is-5-0 ℃.
7. The synthesis method according to claim 1, wherein in the step (2), the dry-basis mass ratio of isobutyryl chloride to alkaline solution is 1.
8. The synthesis method according to claim 1, wherein in the step (3), the liquid separation, washing and liquid separation specifically comprise: standing the reaction solution at-10 deg.C to 0 deg.C for 0-60min, separating water layer to obtain mother liquor, washing the mother liquor with washing solution to pH8-10, standing at-10 deg.C to 0 deg.C to remove water layer, repeating for 2-4 times to obtain diisobutyryl peroxide; the washing liquid is selected from at least one of sodium bicarbonate and sodium carbonate.
9. Diisobutyryl peroxide obtained by the synthesis method according to any one of claims 1 to 8.
10. Use of the diisobutyryl peroxide according to claim 9 for the preparation of polyethylene resins, polyvinyl chloride resins, polyvinyl acetate resins, organic glass.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211024529.8A CN115611795A (en) | 2022-08-25 | 2022-08-25 | Synthesis method of diisobutyryl peroxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211024529.8A CN115611795A (en) | 2022-08-25 | 2022-08-25 | Synthesis method of diisobutyryl peroxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115611795A true CN115611795A (en) | 2023-01-17 |
Family
ID=84857160
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211024529.8A Pending CN115611795A (en) | 2022-08-25 | 2022-08-25 | Synthesis method of diisobutyryl peroxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115611795A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB950978A (en) * | 1960-10-31 | 1964-03-04 | Montedison Spa | Process for preparing diacylperoxides |
| CN109678773A (en) * | 2018-12-13 | 2019-04-26 | 乌鲁木齐市华泰隆化学助剂有限公司 | A kind of preparation method of peroxide -2-ethyl hexanoic acid tert-butyl |
| CN111072542A (en) * | 2019-12-26 | 2020-04-28 | 云南正邦科技有限公司 | Method for continuously producing diisobutyronitrile peroxide by multi-point feeding and intensive mixing |
| CN112300044A (en) * | 2019-12-06 | 2021-02-02 | 广东中准新材料科技有限公司 | Synthesis and purification method of high-purity tert-butyl peroxy-2-ethylhexyl carbonate |
-
2022
- 2022-08-25 CN CN202211024529.8A patent/CN115611795A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB950978A (en) * | 1960-10-31 | 1964-03-04 | Montedison Spa | Process for preparing diacylperoxides |
| CN109678773A (en) * | 2018-12-13 | 2019-04-26 | 乌鲁木齐市华泰隆化学助剂有限公司 | A kind of preparation method of peroxide -2-ethyl hexanoic acid tert-butyl |
| CN112300044A (en) * | 2019-12-06 | 2021-02-02 | 广东中准新材料科技有限公司 | Synthesis and purification method of high-purity tert-butyl peroxy-2-ethylhexyl carbonate |
| CN111072542A (en) * | 2019-12-26 | 2020-04-28 | 云南正邦科技有限公司 | Method for continuously producing diisobutyronitrile peroxide by multi-point feeding and intensive mixing |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102911086B (en) | Preparation method of trifluoro methanesulfonic anhydride | |
| CN113979967B (en) | Method for catalytic synthesis of accelerator CBS by ionic liquid protective agent | |
| US7439404B2 (en) | Process for production of cumene hydroperoxide | |
| CN113582900A (en) | Preparation method of high-purity powdered dibenzoyl peroxide | |
| CN108530383B (en) | Vulcanization accelerator TBBS and continuous production method thereof | |
| CN102369184A (en) | Process for producing perfluoro organic peroxide | |
| CN101947468A (en) | Composite catalyst and application | |
| CN106431887A (en) | Method for preparing trimesic acid | |
| CN115611795A (en) | Synthesis method of diisobutyryl peroxide | |
| CN102731465B (en) | Method for synthesizing epsilon-caprolactone | |
| CN112125825A (en) | Preparation formula of 4' -bromomethyl-2-cyanobiphenyl | |
| CN105646316A (en) | Method for preparing acetic acid solution with low water content and high peracetic acid concentration and consecutive preparation device | |
| CN106349139A (en) | Preparation method of high-purity benzoyl peroxide | |
| WO2023056739A1 (en) | Production process for accelerator dcbs | |
| CN109970793A (en) | A kind of process synthesizing 15 triphenylphosphine salt of carbon | |
| CN115894433A (en) | Process for continuously synthesizing vinyl sulfate crude product | |
| CN102260165B (en) | Method for co-production of citric acid and calcium sulfate dihydrate | |
| CN113845093A (en) | Method for continuously preparing peroxysulfuric acid by using microchannel reactor | |
| CN114713164A (en) | Dibenzothiazole disulfide micro-reaction continuous synthesis system and synthesis method | |
| CN111072542A (en) | Method for continuously producing diisobutyronitrile peroxide by multi-point feeding and intensive mixing | |
| CN113214074A (en) | Method for producing high-purity 3-chloropropionyl chloride by one-pot method | |
| CN112321530A (en) | Preparation method of continuous synthetic rubber vulcanization accelerator CBS | |
| CN112110808A (en) | Preparation method of palladium bis (acetylacetonate) | |
| KR960000015B1 (en) | Enhanced gas-liquid reactions | |
| CN110776477A (en) | Method for preparing DM by oxidizing M with hydrogen peroxide |
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 |