CN100999444A - Method of preparing methyl naphthalene pheol - Google Patents
Method of preparing methyl naphthalene pheol Download PDFInfo
- Publication number
- CN100999444A CN100999444A CN 200610156032 CN200610156032A CN100999444A CN 100999444 A CN100999444 A CN 100999444A CN 200610156032 CN200610156032 CN 200610156032 CN 200610156032 A CN200610156032 A CN 200610156032A CN 100999444 A CN100999444 A CN 100999444A
- Authority
- CN
- China
- Prior art keywords
- naphthol
- zirconium
- sulfuric acid
- purity
- methyl
- 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
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a preparation method of naphthol, with the following steps: add water, naphthylamine and sulfuric acid into Zirconium reactor in order, under 0.9 ~ 1.5 MPa pressures, 180 ~ 200 deg to hydrolyze for 4 to 6 hours to obtain naphthol. The naphthylamine, sulfuric acid and water weight ratio is 1: (0.7 ~ 0.9): (3-4). The naphthylamine purity is 96% to 99.9%, and the naphthol purity of 96% to 99.9%. Referred sulfuric acid is 98wt% concentrated sulfuric acid. The wall of described Zirconium bioreactor is zirconium plant. The invention has a simple process, lower production costs and no tar and coke-generation, belongs to clean production processes.
Description
Technical field
The invention belongs to organic chemistry filed, be specifically related to a kind of preparation method of naphthol.
Background technology
Chinese patent CN1102565C discloses and has a kind ofly prepared the high purity method of naphthol with high-purity methyl naphthylamine, and the material of the inwall of the hydrolysis reactor that this method is used is to ward off lead, so can generate tar after the hydrolysis, must pass through underpressure distillation and remove tar.Technological process is loaded down with trivial details.And use the cost of warding off plumbous material also higher.
Summary of the invention
The purpose of this invention is to provide the preparation method of naphthol that a kind of technological process is simple, production cost is lower.
The technical scheme that realizes the object of the invention is: a kind of preparation method of naphthol, have following steps: in the zirconium reactor, add entry, methyl naphthylamine and sulfuric acid successively, under the pressure of 0.9～1.5Mpa, hydrolysis 4～6h obtains methyl naphthol under 180～200 ℃ the temperature.
The weight ratio of described methyl naphthylamine, sulfuric acid and water is 1: (0.7～0.9): (3～4).The purity of described methyl naphthylamine is 96%～99.9%, and the purity of resulting methyl naphthol is 96%～99.9% after the hydrolysis.Described sulfuric acid is that concentration is the vitriol oil of 98wt%.The inwall of described zirconium reactor is the zirconium plate.
Positively effect of the present invention: the material that (1) hydrolysis reactor inwall of the present invention is adopted is a zirconium, therefore there are not tar and carbonizing matter to generate after the hydrolysis, for the hydrolysis after product of purity lower (for example 96%), sell through promptly can be used as product after the distillation; Can directly enter high tower for the material after the hydrolysis of purity higher (decide according to client's needs, for example 99%～99.9%) and separate (referring to Chinese patent CN1268602C), save the fore-distillation operation, it is simple that technology becomes.(2) only need 8 zirconium pots just can produce 3000 tons methyl naphthol, use the lead pan of warding off of same capability then to need 38, therefore saved the place greatly.(3) adopt when warding off lead pan, for warding off plumbous personnel, also need to carry out the lead discharging of human body, make easily and ward off plumbous personnel's lead poisoning, and contaminate environment, use the zirconium pot then not have this problem, belong to process for cleanly preparing.(4) adopt the zirconium reactor to reduce production costs greatly, producing 1 ton of methyl naphthol equally needs 1.3 tons of raw material methyl naphthylamines with warding off lead pan, uses the zirconium pot then only to need 1.1 tons of raw material methyl naphthylamines, and raw materials cost has reduced.Can also save organic materials expenses such as warding off plumbous expense, paraffin, steam coal expense in post-processing stages in addition.Amount to 1 ton of methyl naphthol of production and can save 4600 yuan.
Table 1
| Unit consumption (ton) | Unit price (unit/ton) | Subtotal (unit) | ||
| Consume with the lead pan production cost | High-purity methyl naphthylamine | 1.3 | 16500 | 21450 |
| Sulfuric acid | 0.84 | 260 | 218.4 | |
| Soda ash | 0.003 | 1650 | 4.95 | |
| The machine material, ward off lead, paraffin | 800 | |||
| The steam coal | 1150 | |||
| The electricity charge | 200 | |||
| Add up to (unit) | 23823.35 | |||
| Consume with zirconium pot production cost | High-purity methyl naphthylamine | 1.1 | 16500 | 18150 |
| Sulfuric acid | 0.84 | 260 | 218.4 | |
| Soda ash | 0.003 | 1650 | 4.95 | |
| The machine material | 150 | |||
| The steam coal | 500 | |||
| The electricity charge | 200 | |||
| Add up to (unit) | 19223.35 |
Embodiment
(embodiment 1).
In the zirconium pot, add 1280kg water, 400kg purity successively and be 96% methyl naphthylamine, add 308kg concentration again and be 98% the vitriol oil, closed the valve of zirconium pot, progressively be warmed up to 190 ℃, pressure in the zirconium pot is raised to 1.1Mpa simultaneously, is incubated 5h under this temperature and pressure, makes hydrolysis reaction complete; Obtain purity and be 96% methyl naphthol 363.6kg, yield is 90.28%.
(embodiment 2).
In the zirconium pot, add 1855kg water, 530kg purity successively and be 97% methyl naphthylamine, add 424kg concentration again and be 98% the vitriol oil, closed the valve of zirconium pot, progressively be warmed up to 180 ℃, pressure in the zirconium pot is raised to 0.9Mpa simultaneously, is incubated 4h under this temperature and pressure, makes hydrolysis reaction complete; Obtain purity and be 97% methyl naphthol 500kg, yield is 93.69%.
(embodiment 3).
In the zirconium pot, add 4200kg water, 1050kg purity successively and be 99% methyl naphthylamine, add 945kg concentration again and be 98% the vitriol oil, closed the valve of zirconium pot, progressively be warmed up to 200 ℃, pressure in the zirconium pot is raised to 1.5Mpa simultaneously, under this temperature and pressure, be incubated 6h, make hydrolysis reaction complete; Material after the hydrolysis is directly sent into high tower separate that to obtain purity be 99% methyl naphthol 1000kg, yield is 94.57%.
(embodiment 4).
In the zirconium pot, add 600kg water, 200kg purity successively and be 99.9% methyl naphthylamine, add 140kg concentration again and be 98% the vitriol oil, closed the valve of zirconium pot, progressively be warmed up to 190 ℃, pressure in the zirconium pot is raised to 1.3Mpa simultaneously, under this temperature and pressure, be incubated 5h, make hydrolysis reaction complete; Material after the hydrolysis is directly sent into high tower separate that to obtain purity be 99.9% methyl naphthol 196.1kg, yield is 97.36%.
Claims (5)
1, a kind of preparation method of naphthol is characterized in that having following steps: add entry, methyl naphthylamine and sulfuric acid in the zirconium reactor successively, under the pressure of 0.9～1.5Mpa, hydrolysis 4～6h obtains methyl naphthol under 180～200 ℃ the temperature.
2, preparation method of naphthol according to claim 1 is characterized in that: the weight ratio of described methyl naphthylamine, sulfuric acid and water is 1: (0.7～0.9): (3～4).
3, preparation method of naphthol according to claim 1, it is characterized in that: the purity of described methyl naphthylamine is 96%～99.9%, the purity of resulting methyl naphthol is 96%～99.9% after the hydrolysis.
4, preparation high purity method of naphthol according to claim 1 is characterized in that: described sulfuric acid is that concentration is the vitriol oil of 98wt%.
5, preparation high purity method of naphthol according to claim 1, it is characterized in that: the inwall of described zirconium reactor is the zirconium plate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610156032 CN100999444A (en) | 2006-12-31 | 2006-12-31 | Method of preparing methyl naphthalene pheol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610156032 CN100999444A (en) | 2006-12-31 | 2006-12-31 | Method of preparing methyl naphthalene pheol |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN100999444A true CN100999444A (en) | 2007-07-18 |
Family
ID=38258279
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200610156032 Pending CN100999444A (en) | 2006-12-31 | 2006-12-31 | Method of preparing methyl naphthalene pheol |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100999444A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101544541B (en) * | 2009-04-30 | 2013-01-02 | 江苏华达化工集团有限公司 | Cyclic utilization method of waste sulfuric acid produced in alpha naphthylamine production |
| CN104557466A (en) * | 2015-01-19 | 2015-04-29 | 河南省商业科学研究所有限责任公司 | Synthesis method of 5-bromine1-naphthol |
-
2006
- 2006-12-31 CN CN 200610156032 patent/CN100999444A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101544541B (en) * | 2009-04-30 | 2013-01-02 | 江苏华达化工集团有限公司 | Cyclic utilization method of waste sulfuric acid produced in alpha naphthylamine production |
| CN104557466A (en) * | 2015-01-19 | 2015-04-29 | 河南省商业科学研究所有限责任公司 | Synthesis method of 5-bromine1-naphthol |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101778944A (en) | Method for the conversion of biomass from renewable raw materials in anaerobic fermenters | |
| CN103113187B (en) | By the method for acetic acid ethanol co-production ethyl acetate | |
| CN101130793A (en) | Novel method for producing fuel alcohol by rice hull and comprehensive utilization of resource | |
| CN101659606A (en) | Method for producing calcium formate by using industrial waste liquid | |
| CN102115764A (en) | Method for producing alcohol by taking anaerobic effluent as ingredient water | |
| CN101407727A (en) | Method for preparing biomass liquefied oil by biomass catalytic liquefaction | |
| WO2016173262A1 (en) | Method for producing cellulosic ethanol by fermenting agricultural and forest biomass waste thick mash | |
| CN101302545B (en) | Production method of acetone-butanol | |
| CN103319346A (en) | Method and device for synthesizing plasticizer by regulating pressure | |
| CN100999444A (en) | Method of preparing methyl naphthalene pheol | |
| CN101633627A (en) | Process for producing 3-(N,N-diallyl)amino-4-p-methoxyacetanilide | |
| CN100532396C (en) | Process for preparing high purity pectin by using apple pomace | |
| CN109456207B (en) | Preparation method of 3-aminopropanol | |
| CN102260230B (en) | Method for preparing furfural by using two-step hydrolysis of biomass | |
| CN103880792A (en) | Method for producing furfural through hydrolysis by using high-pressure two-kettle-cascade acid process | |
| CN101698640A (en) | Method for extracting citric acid | |
| CN110872541A (en) | Method for converting illegal cooking oil into biodiesel | |
| CN101376634B (en) | Non-polluted method for producing o-chloroaniline with ferrous powder as reducer | |
| CN108707064B (en) | Production method for co-producing dimethyl ether by using blast furnace gas | |
| CN102154398A (en) | High-temperature and high-pressure cellulose-to-sugar process | |
| CN107311964B (en) | Method for preparing furfural by liquefying bamboo powder under catalysis of iron phosphate | |
| CN106831323B (en) | Method for preparing chemicals by direct hydrothermal hydrogenation of corncobs | |
| CN101698632B (en) | High-purity 2-ethylene chlorohydrin production method | |
| CN114685245B (en) | System and method for co-production of fuel ethanol and high-grade wine | |
| CN211814390U (en) | Device for producing cellulosic ethanol by using xylose residues |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Open date: 20070718 |