CN107973734A - A kind of preparation method of disuccinic acid peroxide - Google Patents
A kind of preparation method of disuccinic acid peroxide Download PDFInfo
- Publication number
- CN107973734A CN107973734A CN201711234581.5A CN201711234581A CN107973734A CN 107973734 A CN107973734 A CN 107973734A CN 201711234581 A CN201711234581 A CN 201711234581A CN 107973734 A CN107973734 A CN 107973734A
- Authority
- CN
- China
- Prior art keywords
- succinic anhydride
- reaction
- disuccinic acid
- preparation
- acid peroxide
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of preparation method of disuccinic acid peroxide, at 5 ~ 12 DEG C, hydrogen peroxide is set to be reacted with succinic anhydride in aqueous medium, wherein hydrogen peroxide uses aqueous solution, succinic anhydride is 1: 1 ~ 1.7 with hydroperoxidation molar ratio, succinic anhydride is 1: 6 ~ 20 with water inventory molar ratio in reaction system, and the reaction time is 1 ~ 3h, needs to be vigorously stirred in reaction process, after the completion of reaction, stand still for crystals, filter to obtain the final product, the present invention has the characteristics that technique is simple, of low cost.
Description
Technical field
The present invention relates to a kind of preparation method of disuccinic acid peroxide, belong to synthesis technical field.
Background technology
Disuccinic acid peroxide belongs to one kind of diacyl peroxide in organic peroxide, is mainly used as plastics, rubber
Polymerization initiator, bactericidal agent, heavy diesel fuel additive（Improve Cetane number）Deng.
Disuccinic acid peroxide chance light or heated easily decomposition, rubbed, vibrations or shock can cause burning or explosion；With reduction
Vigorous reaction can occur for the contacts such as agent, accelerating agent, organic matter, combustible, there is the danger of combustion explosion.Due to its transportational process
Dangerous and unstability, the producer for selling disuccinic acid peroxide currently on the market are seldom.By patent retrieval, this also there are no
Patent report prepared by chemicals.
The content of the invention
The technical problem to be solved by the invention is to provide a kind of simple, the of low cost disuccinic acid peroxide of technique
Preparation method.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
A kind of preparation method of disuccinic acid peroxide, at 5 ~ 12 DEG C, makes hydrogen peroxide be reacted with succinic anhydride in aqueous medium,
Wherein hydrogen peroxide uses aqueous solution, and succinic anhydride is 1: 1 ~ 1.7 with hydroperoxidation molar ratio, succinic anhydride and reactant
Water inventory molar ratio is 1: 6 ~ 20 in system, and the reaction time is 1 ~ 3h, needs to be vigorously stirred in reaction process, quiet after the completion of reaction
Put crystallization, filter to obtain the final product.
Preferably, succinic anhydride and hydroperoxidation molar ratio are 1: 1.4 ~ 1.7.
Preferably, succinic anhydride and water inventory molar ratio in reaction system are 1: 12 ~ 18.
Preferably, reaction temperature is 7 ~ 10 DEG C.
Preferably, reactant need to stand still for crystals 1 ~ 4h.
Preferably, filtered using vacuum filtration mode, the suction filtration time is 0.5 ~ 2h.
Reaction equation is as follows：
2CH2COOOCCH2+H2O2→HOOCCH2CH2COO-OOCCH2CH2COOH+ H2O
Disuccinic acid peroxide assay can refer to the measure iodimetric titration of GB/T 32102-2015 organic peroxide contents.
Instrument：250mL iodine flasks；50mL minimum scale 0.1mL burets；Sensibility reciprocal 0.0001g assay balances.
Reagent：Glacial acetic acid；Dichloromethane；Saturated solution of potassium iodide；0.1mol/L sodium thiosulfate standard solutions；Starch refers to
Show agent.
Analytical procedure：
1st, in the iodine flask for measuring 20mL glacial acetic acids injection 250mL, 0.6 ~ 0.8g samples is accurately weighed, are accurate to 0.0001g, are added
Enter in iodine flask；
2nd, toward addition 10mL dichloromethane in iodine flask, and bottle stopper is stoppered, vibration is completely dispersed sample；
3rd, saturated solution of potassium iodide 5mL is added, is stoppered bottle stopper, lucifuge of opening in dark place at room temperature after shaking up stands 15min；
4th, in iodine flask add 50mL water, be titrated to sodium thiosulfate standard solution it is light yellow, then add 1mL ~ 2mL shallow lake
Powder indicator, it is terminal to continue to be titrated to colourless, record consumption sodium thiosulfate volume；
5th, blank test is done.
As a result calculate：
Disuccinic acid peroxide content calculates as follows：
In formula：
W-disuccinic acid peroxide content, %；
The volume of V1-sample consumption sodium thiosulfate standard solution, mL；
The volume of V2-blank sample consumption sodium thiosulfate standard solution, mL；
The amount of substance concentration of c-sodium thiosulfate standard solution, mol/L；
The molal weight of M-disuccinic acid peroxide, 234.16g/mol；
The quality of m-weigh disuccinic acid peroxide, g.
The beneficial effect that the present invention is reached：The present invention is mainly carried by controlling reaction temperature and the proportioning of reactant
High reaction yield, reaction temperature is high, and hydrolysis easily occurs for succinic anhydride；Reaction temperature is low, and reaction rate is slow, product yield
It is relatively low.When the timing of succinic anhydride dosage one, hydrogen peroxide use is excessive or very few, and product yield is all than relatively low, hydrogen peroxide
Dosage is very few, and the non-complete oxidation of succinic anhydride, hydrogen peroxide use is excessive, and peroxidization can occur for succinic anhydride, produce
Acid.Need to add pure water in reaction process, the excessive reactant concentration of pure water addition reduces, is unfavorable for oxidation reaction, on the contrary easily makes
Succinic anhydride hydrolyzes；When pure water amount is less, easily occur side reaction, disuccinic acid peroxide decompose compared with Gao Shiyi in temperature and
Combustion explosion, it is impossible to using high temperature drying mode, moisture is removed using the method for vacuum filtration under normal circumstances, the present invention provides
Preparation method have the characteristics that technique is simple, of low cost.
Embodiment
The invention will be further described below.Following embodiments are only used for the technical side for clearly illustrating the present invention
Case, and be not intended to limit the protection scope of the present invention and limit the scope of the invention.
Embodiment 1：
Take 30% hydrogen peroxide 500g, pure water 500mL, succinic anhydride 300g to sequentially add in three-necked flask, flask is placed on frozen water
In bath, start stirring, control water-bath reacts 2h at 9 DEG C.After the completion of reaction, stop stirring and stand still for crystals 3h at 10 DEG C.Will knot
Brilliant liquid vacuum filtration, filter cake 10 DEG C of pure waters 3 times, suction filtration 1h is up to product.
Embodiment 2：
Take 30% hydrogen peroxide 350g, pure water 700mL, succinic anhydride 300g to sequentially add in three-necked flask, flask is placed on frozen water
In bath, start stirring, control water-bath reacts 2h at 9 DEG C.After the completion of reaction, stop stirring and stand still for crystals 3h at 10 DEG C.Will knot
Brilliant liquid vacuum filtration, filter cake 10 DEG C of pure waters 3 times, suction filtration 1h is up to product.
Embodiment 3：
Take 30% hydrogen peroxide 460g, pure water 540mL, succinic anhydride 300g to sequentially add in three-necked flask, flask is placed on frozen water
In bath, start stirring, control water-bath reacts 2h at 9 DEG C.After the completion of reaction, stop stirring and stand still for crystals 2h at 10 DEG C.Will knot
Brilliant liquid vacuum filtration, filter cake 10 DEG C of pure waters 3 times, suction filtration 1h is up to product.
Embodiment 4：
Take 30% hydrogen peroxide 550g, pure water 100mL, succinic anhydride 300g to sequentially add in three-necked flask, flask is placed on frozen water
In bath, start stirring, control water-bath reacts 3h at 9 DEG C.After the completion of reaction, stop stirring and stand still for crystals 1h at 10 DEG C.Will knot
Brilliant liquid vacuum filtration, filter cake 10 DEG C of pure waters 3 times, suction filtration 1h is up to product.
Embodiment 5：
Take 30% hydrogen peroxide 570g, pure water 300mL, succinic anhydride 300g to sequentially add in three-necked flask, flask is placed on frozen water
In bath, start stirring, control water-bath reacts 2h at 9 DEG C.After the completion of reaction, stop stirring and stand still for crystals 3h at 10 DEG C.Will knot
Brilliant liquid vacuum filtration, filter cake 10 DEG C of pure waters 3 times, suction filtration 2h is up to product.
Embodiment 6：
Take 30% hydrogen peroxide 500g, pure water 500mL, succinic anhydride 300g to sequentially add in three-necked flask, flask is placed on frozen water
In bath, start stirring, 2h is reacted in control water-bath at 5 DEG C.After the completion of reaction, stop stirring and stand still for crystals 3h at 10 DEG C.Will knot
Brilliant liquid vacuum filtration, filter cake 10 DEG C of pure waters 3 times, suction filtration 1.5h is up to product.
Embodiment 7：
Take 30% hydrogen peroxide 500g, pure water 700mL, succinic anhydride 300g to sequentially add in three-necked flask, flask is placed on frozen water
In bath, start stirring, control water-bath reacts 1h at 9 DEG C.After the completion of reaction, stop stirring and stand still for crystals 2h at 10 DEG C.Will knot
Brilliant liquid vacuum filtration, filter cake 10 DEG C of pure waters 3 times, suction filtration 0.5h is up to product.
Disuccinic acid peroxide content see the table below：
Table 1：Disuccinic acid peroxide content in embodiment
| 30% hydrogen peroxide gross weight g | Pure water g | Succinic anhydride g | 100% hydrogen peroxide and succinic anhydride molar ratio | Reaction system water inventory and succinic anhydride molar ratio | Active o content % | |
| Embodiment 1 | 500 | 500 | 300 | 1.47 | 15.74 | 75.62 |
| Embodiment 2 | 350 | 700 | 300 | 1.03 | 17.50 | 60.18 |
| Embodiment 3 | 460 | 540 | 300 | 1.35 | 15.96 | 65.57 |
| Embodiment 4 | 550 | 100 | 300 | 1.62 | 8.98 | 57.63 |
| Embodiment 5 | 570 | 300 | 300 | 1.68 | 12.94 | 70.74 |
| Embodiment 6 | 500 | 500 | 300 | 1.47 | 15.74 | 58.34 |
| Embodiment 7 | 500 | 700 | 300 | 1.47 | 19.44 | 50.56 |
The above is only the preferred embodiment of the present invention, it is noted that is come for those skilled in the art
Say, without departing from the technical principles of the invention, some improvement and deformation can also be made, these are improved and deformation also should
It is considered as protection scope of the present invention.
Claims (6)
1. a kind of preparation method of disuccinic acid peroxide, it is characterized in that, at 5 ~ 12 DEG C, make hydrogen peroxide with succinic anhydride in water
Reacted in medium, wherein hydrogen peroxide uses aqueous solution, and succinic anhydride is 1: 1 ~ 1.7 with hydroperoxidation molar ratio, fourth two
Acid anhydrides is 1: 6 ~ 20 with water inventory molar ratio in reaction system, and the reaction time is 1 ~ 3h, needs to be vigorously stirred in reaction process, instead
After the completion of answering, stand still for crystals, filter to obtain the final product.
2. a kind of preparation method of disuccinic acid peroxide according to claim 1, it is characterized in that, succinic anhydride and peroxidating
Hydrogen reaction molar ratio is 1: 1.4 ~ 1.7.
3. according to a kind of preparation method of disuccinic acid peroxide of claim 1-2 any one of them, it is characterized in that, succinic anhydride
It is 1: 12 ~ 18 with water inventory molar ratio in reaction system.
4. a kind of preparation method of disuccinic acid peroxide according to claim 3, it is characterized in that, reaction temperature is 7 ~ 10
℃。
5. a kind of preparation method of disuccinic acid peroxide according to claim 3, it is characterized in that, reactant need to be stood still for crystals
1~4h。
6. a kind of preparation method of disuccinic acid peroxide according to claim 3, it is characterized in that, using vacuum filtration mode
Filtered, the suction filtration time is 0.5 ~ 2h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711234581.5A CN107973734A (en) | 2017-11-30 | 2017-11-30 | A kind of preparation method of disuccinic acid peroxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711234581.5A CN107973734A (en) | 2017-11-30 | 2017-11-30 | A kind of preparation method of disuccinic acid peroxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107973734A true CN107973734A (en) | 2018-05-01 |
Family
ID=62008469
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711234581.5A Pending CN107973734A (en) | 2017-11-30 | 2017-11-30 | A kind of preparation method of disuccinic acid peroxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107973734A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4129517A (en) * | 1976-11-30 | 1978-12-12 | Sterling Drug Inc. | Aqueous peroxy-containing concentrate |
| CN1067882A (en) * | 1992-05-08 | 1993-01-13 | 中国人民解放军沈阳军区后勤部卫生防疫队 | A kind of preparation method of solid-state amyldiacid peroxide |
| CN102093276A (en) * | 2010-12-01 | 2011-06-15 | 中昊晨光化工研究院 | Preparation method peroxided succinic acid |
-
2017
- 2017-11-30 CN CN201711234581.5A patent/CN107973734A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4129517A (en) * | 1976-11-30 | 1978-12-12 | Sterling Drug Inc. | Aqueous peroxy-containing concentrate |
| CN1067882A (en) * | 1992-05-08 | 1993-01-13 | 中国人民解放军沈阳军区后勤部卫生防疫队 | A kind of preparation method of solid-state amyldiacid peroxide |
| CN102093276A (en) * | 2010-12-01 | 2011-06-15 | 中昊晨光化工研究院 | Preparation method peroxided succinic acid |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103666456B (en) | Boron-dipyrromethene fluorescence probes, and making method and application thereof | |
| CN104529957A (en) | Preparation method of 2,5-furandicarboxylate | |
| CN103913441B (en) | Rhodamine B fluorescence sensor, preparation and application thereof | |
| CN102659677A (en) | Fluorescent molecular probe for detecting sulfite ions through naked eyes and fluorescence ratio as well as synthesis and application thereof | |
| CN109336815B (en) | Two-photon fluorescent probe for detecting hypochlorous acid in intracellular endoplasmic reticulum | |
| CN110372632B (en) | Fluorescent probe molecule for rapidly identifying hypochlorite ions and preparation method and application thereof | |
| Brown et al. | Phytic acid: an analytical investigation | |
| CN104803398A (en) | Non-caking salt composition, preparation process and use thereof | |
| CN107022060A (en) | A kind of preparation technology of the electronic grade hydrogenated bisphenol A epoxide resin of high-purity | |
| CN109824726A (en) | A kind of preparation method, nonaqueous electrolytic solution and the battery of the double oxalic acid lithium phosphates of difluoro | |
| CN107973734A (en) | A kind of preparation method of disuccinic acid peroxide | |
| CN109400563B (en) | Hypochlorous acid fluorescent probe and preparation method and application thereof | |
| CN112375006B (en) | Method for improving conversion rate in production of iminodisuccinate | |
| CN102093276B (en) | Preparation method peroxided succinic acid | |
| CN103131205B (en) | Rhodamine fluorochrome and preparation method and application of rhodamine fluorochrome | |
| Wassermann | 127. Homogeneous catalysis of diene syntheses. A new type of third-order reaction | |
| CN102323179A (en) | Method for detecting sulfur dioxide in desulfurized gypsum | |
| CN104276981A (en) | Method of synthesis of azo compounds | |
| Hosahalli et al. | Kinetics and mechanism of ruthenium (III) catalyzed oxidation of chloromphenicol—An antibiotic drug by diperiodatocuprate (III) in aqueous alkaline medium | |
| CN108884027A (en) | The method for preparing 3- methylthiopropionaldehyde | |
| CN107628933A (en) | A kind of continuous production technology that the acetone of 1 methoxyl group 2 is synthesized by the propyl alcohol direct dehydrogenation of 1 methoxyl group 2 | |
| CN106046318B (en) | A kind of method for reducing the total chlorine of epoxy resin | |
| CN103420351B (en) | A kind of production technique of Efficacious Disinfeitant | |
| Lineweaver | Acceleration by electrolytes of alkaline de-esterification of pectin | |
| CN112159331B (en) | Storage method for improving effective content of iminodisuccinate product and application thereof |
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 | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180501 |