CN1024343C - Process for refining methyl naphthol at low temp. - Google Patents
Process for refining methyl naphthol at low temp. Download PDFInfo
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- CN1024343C CN1024343C CN 90102814 CN90102814A CN1024343C CN 1024343 C CN1024343 C CN 1024343C CN 90102814 CN90102814 CN 90102814 CN 90102814 A CN90102814 A CN 90102814A CN 1024343 C CN1024343 C CN 1024343C
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- methyl naphthol
- naphthol
- thick methyl
- fused
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Abstract
The present invention relates to a process for refining methyl naphthol at low temperature, which comprises: controlling the detemperature rate and range of methyl naphthol in a low-temperature refining tank to separate out relatively pure methyl naphthol crystals, then, raising temperature at certain speed to increase the methyl naphthol content in distillate in a gradient to obtain refined methyl naphthol. The present invention has the advantages of high product purity, little loss and no three-waste pollution, and solves the problems of high energy consumption and poor product quality of a distillation purification process and the solvent recovery, product drying, etc. problems of a solvent refining method.
Description
The present invention relates to the method for purification of Chemicals, specifically, it is a kind of technology of refining methyl naphthol at low temp.
Methyl naphthol also claims 1-naphthols or naphthyl alcohol, and it is the important intermediate of a kind of dyestuff, agricultural chemicals.Wherein, it main application is the synthetic wide spectrum agricultural chemicals " SevinCarbaryl " of producing efficient, low toxicity, low residue.But the methyl naphthol of low-purity be can not produce high-quality agricultural chemicals " SevinCarbaryl ", and owing to have harmful composition in the methyl naphthol of low-purity, is brought in the agricultural chemicals " SevinCarbaryl ", with harm user's health.Traditional methyl naphthol production technique, system adopts distillation method to purify, its shortcoming is distillation having relatively high expectations to equipment, azeotropism usually takes place during distillation, bring operational difficulty, the energy consumption height of simultaneous distillation method, yield quality (purity) low, product are relatively poor, generally only between 92-95%, can't satisfy the requirement of producing high quality agricultural chemicals " SevinCarbaryl ".In prior art, United States Patent (USP) has disclosed a kind of technology with tetracol phenixin purification methyl naphthol for No. 380224, according to this method, can obtain the methyl naphthol of purity 99.7%, but this technology exists solvent recuperation, product drying and solvent to problems such as human body murders by poisoning.The inventor is by research repeatedly, discovery is when low temperature, and thick methyl naphthol is a kind of eutectic mixture, and its formation is by main component methyl naphthol and minor consistuent ethyl naphthol, and, also may contain a spot of other impurity and be mixed in the eutectic mixture according to the difference of the production technique of methyl naphthol.When temperature reduces, its main component methyl naphthol will be separated out with pure crystal structure, minor consistuent ethyl naphthol and other impurity then accumulate in the remaining raffinate, principle according to solid-liquid equilibrium, contain the raffinate of impurity and less important composition by effective discharging, the purity of methyl naphthol is risen in gradient, reach methyl naphthol content 〉=99%, zero pour 〉=93.6 ℃ can be satisfied the requirement of producing high-quality " SevinCarbaryl " agricultural chemicals fully.The present invention finishes on the basis of above-mentioned discovery.
So, the object of the present invention is to provide a kind of technology of refining methyl naphthol at low temp.
The objective of the invention is to finish in the following manner: the cooling rate and the scope that are controlled at thick methyl naphthol in the low-temperature purifying method groove, material is separated out with purer methyl naphthol crystallization in groove, then, heat up with certain speed again, make that the content of methyl naphthol raises in gradient in the effluent.It is characterized in that:
1) with the thick methyl naphthol fast cooling of fused to its fusing point, then,, preferably be cooled to its below fusing point 10 °-25 ℃ with 1 ° of-3 ℃ of control per hour per hour to lower the temperature 0.5 °-5 ℃;
2) the thick methyl naphthol that will solidify is with 1 ° of-5 ℃ of speed per hour, preferably, is warming up to the methyl naphthol fusion again of solidifying with 2 ° of-4 ℃ of speed control per hour, then
3) the smart methyl naphthol of the fused of the different melting ranges of step emission;
4) last, discharging is in homothermic purified methyl naphthol.
The purity that it is characterized in that described thick methyl naphthol is not less than 60%(weight at least).
It is characterized in that preferably being 1 °-2 ℃ with the thick methyl naphthol fast cooling of fused 0.5 °-5 ℃ to its fusing point.
It is characterized in that with the thick methyl naphthol of fused at 10 minutes to 1 hour fast coolings to its fusing point.
Its feature is that also described constant temperature time is 0.5-8 hour, preferably is 1.5-3 hour.
Advantage of the present invention is tangible, refining not only energy consumption is low than traditional distillation for low-temperature purifying method of the present invention, and because methyl naphthol resistance to oxidation not is serious through the pyrogenic distillation loss, yield is lower, the quality of product (purity) is lower, can't satisfy the requirement of producing high quality agricultural chemicals " SevinCarbaryl ".And adopt technology of the present invention, not only the refining purity of methyl naphthol can reach more than 99%, zero pour 〉=93.6 ℃, has met the standard of producing high-quality agricultural chemicals, dyestuff and pharmaceutical production fully.Simultaneously, its recovery rate is apparently higher than distillation method technology, and the refining methyl naphthol of producing 1 ton of 99% purity of technology of the present invention only consumes 1.15 tons of thick methyl naphthols.In addition, the present invention is that physical method is refining, and no by product produces and do not have " three wastes " and pollute generation.
Below, the present invention will be described in detail in conjunction with concrete enforcement, so that advantage of the present invention is more obvious.
Embodiment 1
With 90.15 ℃ of purity of zero pour of 100 parts of weight is 92%(weight) the thick methyl naphthol of fused be added in the refinery pit of strap clamp cover, during 30 minutes, be cooled to 92 ℃ apace, then, be cooled to 70 ℃ with 1 ° of-5 ℃ of control per hour, then be warming up to 73.9 ℃ ± 1 ℃, and discharge 10 parts of the thick methyl naphthols (weight) of this melting range with 2 °-4 ℃ speed per hour; Then be warming up to 84.5 ℃ ± 1 ℃ again, and discharge 19 parts of the thick methyl naphthols (weight) of this melting range; Be warming up to 89.4 ℃ ± 1 ℃ again, and discharge 27.5 parts of the thick methyl naphthols (weight) of this melting range, last, material discharges 43.5 parts of (weight) purified methyl naphthols (purity 〉=95% zero pour is 92.1 ℃) 92 ℃ ± 1 ℃ constant temperature two hours.
Embodiment 2
The thick methyl naphthol of fused of the fusing point that obtains among the embodiment 1 with 100 parts of weight 92.1 ℃ (purity 〉=95%) is added in the refinery pit of strap clamp cover, apace at 1 hour internal cooling to 93 ℃, be cooled to 93 ℃ with 2 ° of-4 ℃ of controls per hour then, be warming up to 80.6 ℃ ± 1 ℃ with 1 ° of-5 ℃ of control per hour then, and discharge 6.5 parts of the thick methyl naphthols (weight) of this melting range; Then, be warming up to 88.9 ℃ ± 1 ℃ again, and discharge 22 parts of the thick methyl naphthols (weight) of this melting range; Then, be warming up to 92.15 ℃ again, and discharge 27.7 parts of the methyl naphthols (weight) of this melting range, last, material is 93.6 ± 1 ℃ of constant temperature 1 hour, and discharges the refining methyl naphthol (purity 〉=99%, zero pour are 93.65 ℃) of 43.8 parts (weight).
Embodiment 3
The thick methyl naphthol of fused of 81.65 ℃ at the zero pour of 100 parts of weight is added in the refinery pit of strap clamp cover, apace at 10 minutes internal cooling to 82 ℃, then be cooled to 50 ℃ with 0.5 ° of-5 ℃ of speed per hour, then be warming up to 51.5 ℃ ± 1 ℃, and discharge 16.6 parts of the thick methyl naphthols (weight) of this melting range with 1 ° of-3 ℃ of speed per hour; Then be warming up to 67.5 ℃ ± 1 ℃, and discharge 16.5 parts of the thick methyl naphthols (weight) of this melting range.Be warming up to 80.2 ℃ ± 1 ℃ again, and discharge 19.8 parts of the thick methyl naphthols (weight) of this melting range; Then, be warming up to 86.1 ℃ ± 1 ℃ again, and discharge 14.3 parts of the thick methyl naphthols (weight) of this melting range; At last, 90.9 ℃ ± 1 ℃ constant temperature three hours, and 32.8 parts of (weight) (purity 〉=90% zero pour are 90.9 ℃) of smart methyl naphthol of discharging this melting range
Embodiment 4
The thick methyl naphthol of fused of 69.1 ℃ at the zero pour of 100 parts of weight is added to the refinery pit of strap clamp cover, in 20 minutes fast coolings to 70 ℃; Then, be cooled to 50 ℃ with 1-3 ℃ speed per hour; Then enter the control temperature rise period, be warming up to 53.7 ℃ ± 1 ℃ with 2-4 ℃ of speed per hour, and discharge 28.36 parts of the thick methyl naphthols (weight) of this melting range; Then, be warming up to 65.3 ℃ ± 1 ℃ and discharge 37.65 parts of the thick methyl naphthols (weight) of this melting range; At last, be warming up to 82 ℃ ± 1 ℃ constant temperature two hours, side by side 33.98 parts of (weight) (zero pour are 82.1 ℃) of the methyl naphthol after the spermiation system.
Claims (7)
1, a kind of refining methyl naphthol technology is characterized in that
1), with the thick methyl naphthol fast cooling of fused to its more than fusing point, then, be cooled to its below fusing point 10 °-25 ℃ with 0.5 ° of-5 ℃ of control of per hour lowering the temperature;
2), the thick methyl naphthol that will solidify is warming up to the thick methyl naphthol fusion again of solidifying with 1 ° of-5 ℃ of speed speed control per hour; Then
3), the thick methyl naphthol of fused of the different melting ranges of step emission;
4), last, discharging is in homothermic purified methyl naphthol.
2, technology as claimed in claim 1 is characterized in that
1), with the thick methyl naphthol fast cooling of fused to its more than fusing point, then, be cooled to its below fusing point 10 °-25 ℃ with 1 ° of-5 ℃ of control of per hour lowering the temperature;
2), the thick methyl naphthol that will solidify is warming up to the thick methyl naphthol fusion again of solidifying with 2 ° of-4 ℃ of speed speed control per hour;
3), the thick methyl naphthol of fused of the different melting ranges of step emission;
4), last, discharging is in homothermic purified methyl naphthol.
3, technology as claimed in claim 1 or 2 is characterized in that the purity of the thick methyl naphthol of described fused fast cooling is not less than 60%(weight at least).
4, technology as claimed in claim 1 or 2 is characterized in that the thick methyl naphthol fast cooling of fused 0.5 °-5 ℃ to its fusing point.
5, technology as claimed in claim 4 is characterized in that the thick methyl naphthol fast cooling of fused 1 °-2 ℃ to its fusing point.
6, technology as claimed in claim 1 or 2, it is characterized in that with the thick methyl naphthol of fused at 10 everys minute ands second to 1 hour fast cooling to its fusing point.
7, technology as claimed in claim 1 or 2 is characterized in that described constant temperature time is 0.5-8 hour, preferably is 1.5-3 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90102814 CN1024343C (en) | 1990-03-16 | 1990-03-16 | Process for refining methyl naphthol at low temp. |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90102814 CN1024343C (en) | 1990-03-16 | 1990-03-16 | Process for refining methyl naphthol at low temp. |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1054971A CN1054971A (en) | 1991-10-02 |
| CN1024343C true CN1024343C (en) | 1994-04-27 |
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ID=4877701
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 90102814 Expired - Fee Related CN1024343C (en) | 1990-03-16 | 1990-03-16 | Process for refining methyl naphthol at low temp. |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1024343C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1102566C (en) * | 1999-09-28 | 2003-03-05 | 常州市樊达化工有限公司 | Process for industrially preparing very-high-purity 1-naphthol |
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1990
- 1990-03-16 CN CN 90102814 patent/CN1024343C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1054971A (en) | 1991-10-02 |
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