CN106608817A - Production technology of p-methoxybenzoic acid - Google Patents
Production technology of p-methoxybenzoic acid Download PDFInfo
- Publication number
- CN106608817A CN106608817A CN201510754866.6A CN201510754866A CN106608817A CN 106608817 A CN106608817 A CN 106608817A CN 201510754866 A CN201510754866 A CN 201510754866A CN 106608817 A CN106608817 A CN 106608817A
- Authority
- CN
- China
- Prior art keywords
- methoxybenzoic acid
- acetic acid
- production technology
- water
- acid
- 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
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/16—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation
- C07C51/21—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen
- C07C51/255—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of compounds containing six-membered aromatic rings without ring-splitting
- C07C51/265—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of compounds containing six-membered aromatic rings without ring-splitting having alkyl side chains which are oxidised to carboxyl groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/18—Preparation of ethers by reactions not forming ether-oxygen bonds
- C07C41/26—Preparation of ethers by reactions not forming ether-oxygen bonds by introduction of hydroxy or O-metal groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/27—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation
- C07C45/32—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen
- C07C45/33—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of CHx-moieties
- C07C45/34—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of CHx-moieties in unsaturated compounds
- C07C45/36—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of CHx-moieties in unsaturated compounds in compounds containing six-membered aromatic rings
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention discloses a production technology of p-methoxybenzoic acid. The p-methoxybenzoic acid is an important chemical product. The production technology comprises (1) aerobic oxidation of PCME, (2) recovery of acetic acid, (3) catalyst recovery, (4) oil layer treatment, and (5) preparation of p-methoxybenzoic acid through anisyl acetate hydrolysis.
Description
1st, reaction principle
With acetic acid as solvent, using mixed catalyst, under Halogen catalyst system and catalyzing, air is used（Oxygen）Catalysis oxygen
Change is reacted methoxy toluene, prepares P-methoxybenzal-dehyde, P-methoxybenzyl alcohol, acetic acid fennel ester
And P-methoxybenzoic acid, while generating byproduct sulfite and sodium acetate.
（1）P-methoxybenzal-dehyde
（2）P-methoxybenzoic acid
（3）Acetic acid fennel ester
（4）P-methoxybenzyl alcohol
2nd, technical process
（1）Dioxygen oxidation PCME
Cobalt acetate, chromium acetate and cerous acetate are put in stills for air blowing as catalyst, and acetic acid, steam heating
To 70-90 DEG C, after stirring and dissolving, add to methoxy toluene（PCME）, 100-120 DEG C is steam heated to,
It is passed through air（Oxygen）Reaction 2h.
（2）Acetic acid is reclaimed
After reaction to be oxidized terminates, reactant liquor is extruded, proceed to distillation still.140 DEG C are steam heated to, are steamed
Acetic acid reuse to catalyst arrangement step, gained is evaporated into bottom and is washed with water, stratification obtains oil phase
With water phase.
（3）Catalyst is reclaimed
Gained water is mutually filtered, the filtrate containing catalyst, and a small amount of solid waste containing organic matter is produced
S2-1, filtrate is transferred to catalyst and reclaims kettle, and 105-112 DEG C of distillation is warming up at ambient pressure, distills out containing second
The vapor of acid, is back to washing Fen Ye workshop sections, and it is catalyst to evaporate bottom, is transferred in dissolution kettle, adds acetic acid,
In 70-90 DEG C, stirring and dissolving, then reuse is to oxidation operation.
（4）Formation treatment
A point liquid gained oil phase is transferred in distillation still, natrium carbonicum calcinatum is added, is stirred in 70-75 DEG C after 30min, vacuum distillation to kettle temperature ~ 120 DEG C, cut is P-methoxybenzal-dehyde and acetic acid fennel ester crude product, and evaporating bottom is
Sodium anisate crude product, while waste gas G2-2 can be produced.
（5）Prepare P-methoxybenzoic acid
Bottom will be evaporated and add water dissolves, 90-95 DEG C of filtration will be heated to after stirring 30min, obtain filtrate and filter residue
（S2）, filtrate is neutralized in 70-75 DEG C with sulfuric acid, then Jing filters to obtain P-methoxybenzoic acid, and containing steam
With the waste gas G2-3 of carbon dioxide, filtrate stands at normal temperatures again, obtains byproduct sulfite and containing a small amount of
The waste water W2-1 of sulfuric acid.
Rectifying prepares P-methoxybenzal-dehyde and acetic acid fennel ester cut is transferred to rectifying still at 60-140 DEG C, and rectifying is carried out under 1-10mmHg, obtains cut to methoxyl group
Benzaldehyde and cut acetic acid fennel ester and tar S2-3；
（6）Acetic acid fennel ester hydrolysis prepare P-methoxybenzyl alcohol
NaOH, acetic acid fennel ester and water are added in hydrolysis kettle, 60-80 DEG C is steam heated to, is reacted
To sodium acetate and P-methoxybenzyl alcohol crude product.
Stratification, oil phase add acetic acid and water to be washed after stratification, oil phase and water phase are obtained again,
Oil phase adds NaOH and water washing, and stratification obtains again oil phase and water phase, and oil phase is transferred to essence
Kettle is evaporated, at 120 DEG C, rectifying is carried out under 3-5mmHg, obtain P-methoxybenzyl alcohol and tar S2-4.
The water that the water phase that twice washing point liquid is obtained is obtained with standing point liquid is added to acetic acid, and Jing is filtered and obtained byproduct three
（7）Hydrated sodium acetate, and the waste water containing acetic acid and P-methoxybenzyl alcohol.
Material balance
Claims (2)
1. a kind of P-methoxybenzoic acid production technology.
2. the material composition and proportioning of P-methoxybenzoic acid production process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510754866.6A CN106608817A (en) | 2015-11-09 | 2015-11-09 | Production technology of p-methoxybenzoic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510754866.6A CN106608817A (en) | 2015-11-09 | 2015-11-09 | Production technology of p-methoxybenzoic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106608817A true CN106608817A (en) | 2017-05-03 |
Family
ID=58615327
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510754866.6A Pending CN106608817A (en) | 2015-11-09 | 2015-11-09 | Production technology of p-methoxybenzoic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106608817A (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103936567A (en) * | 2014-05-04 | 2014-07-23 | 宿迁科思化学有限公司 | Co-production method of preparing corresponding alcohol, ester, aldehyde and acid by oxidizing p-methoxyl methylbenzene by oxygen |
-
2015
- 2015-11-09 CN CN201510754866.6A patent/CN106608817A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103936567A (en) * | 2014-05-04 | 2014-07-23 | 宿迁科思化学有限公司 | Co-production method of preparing corresponding alcohol, ester, aldehyde and acid by oxidizing p-methoxyl methylbenzene by oxygen |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170503 |
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| WD01 | Invention patent application deemed withdrawn after publication |