CN100497319C - Rectifying method for methyl benzotrizole - Google Patents
Rectifying method for methyl benzotrizole Download PDFInfo
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- CN100497319C CN100497319C CNB2006100388915A CN200610038891A CN100497319C CN 100497319 C CN100497319 C CN 100497319C CN B2006100388915 A CNB2006100388915 A CN B2006100388915A CN 200610038891 A CN200610038891 A CN 200610038891A CN 100497319 C CN100497319 C CN 100497319C
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Abstract
The methyl benzotrizole rectifying process includes setting the oil phase obtained in the methyl benzotrizole producing process in dewatering caldron, heating to eliminate water from the oil phase at normal pressure and negative pressure, rectifying the dewatered material to collect the fraction of methyl benzotrizole under heating and negative condition so as to obtain the rectified methyl benzotrizole product. The present invention has shortened methyl benzotrizole producing period, low power consumption, low production cost, less waste gas and waste water exhaust, and the product has purity over 99.7 %, water content lower than 0.05 %, ash content lower than 0.03 %, smelting point of 78-85 deg.c, high quality and yield over 98 %.
Description
Technical field
The present invention relates to purifying technique field, especially to the rectificating method of tolyltriazole to fine chemical product.
Background technology
In the Chemicals production process, because the multistep chemical reaction of last stage technology, cause the existence of the various organic and inorganic impurity of Chemicals and influence the quality of the finished product.With regard to the production of tolyltriazole, in order to improve the quality of products, reduce and consume, improve product yield, adopted in the past and the tolyltriazole intermediate is carried out the distillatory method purify, because distillation process is to utilize a still kettle and condenser to form, by≤210 ℃ the temperature and the simple procedures of purifying under-0.09Mpa negative pressure, finished product that its distillation receives does not have accurately to collect for 175-180 ℃ according to the boiling point of finished product.In still-process so long as≤all organic and inorganic things of 210 ℃ all enter in the finished product, cause finished product purity not high, directly influence the quality of finished product, can only reach purity less than 90% by distillatory final product quality index, moisture content is less than 0.3%, ash is less than 0.05%, and fusing point is 73-80 ℃.And leftover materials are more in the distillation test residue, and the unit product yield is descended.
Improve in order to ensure the raising of tolyltriazole quality product, yield, can guarantee Chemical Manufacture safety again, should adopt rectification and purification technology the collection of tolyltriazole finished product.
Summary of the invention
What the present invention will solve is exactly the existing problem of above-mentioned existing tolyltriazole production technique, for people provide a kind of rectificating method of tolyltriazole, to guarantee to improve the quality and the yield of tolyltriazole product.
The present invention adopts technical scheme as follows:
Oil phase intermediate in the tolyltriazole production process is placed in the dehydration still, in heating, go down except that the moisture content in the oil phase intermediate at normal pressure and negative pressure respectively, then dehydrated material is carried out rectifying, the finished product fraction is gathered in heating under the condition of negative pressure according to tolyltriazole, obtains the tolyltriazole finished product of rectifying.
The dehydration of aforementioned normal pressure be in temperature in the kettle＜150 ℃, still chuck vapor pressure is 4-6Kg/cm
2The steam heating condition under carry out, dewatering is 3-4 hour.
When observing by looking tube that the negative pressure dehydration finishes when having a small amount of tolyltriazole to invest visor.
After dehydration finishes, under the condition of rectifying tower vacuum index less than 100Pa, the interior temperature of rectifying still is at the uniform velocity heated up, when the rectifying temperature in the kettle rises to 170-180 ℃, when the rectifying tower temperature rises to 120-130 ℃, made in the still feed back 0.5-1 hour, when liquid material in the still is converted to when light yellow by red-brown or yellow, reflux and finish, receive foreshot; When the fraction color by light yellow to when white, begin to gather the finished product fraction; The collection of finished product fraction is gathered after cut after finishing again.
When the rectifying still jacket temperature rises to more than 160 ℃, should slow down heat-up rate, make temperature in the kettle and jacket temperature keep≤40 ℃ the temperature difference.
The finished product fraction receives the still temperature and should be controlled at≤and 110 ℃.
When the collection finished product heated up in a steamer, the rectifying tower vacuum should be less than 100Pa, and the tower temperature is between 125-135 ℃, and should make the temperature of constant temperature water tank remain between 92-98 ℃ this moment.
When the collection finished product heats up in a steamer, should control the interior temperature of charge of rectifying still between 175-198 ℃, the rectifying tower vacuum is less than 100Pa, and the temperature that the finished product fraction receives in the still remains on 90-110 ℃.
When gathering finished product and heat up in a steamer, looking when observing fraction in the tube and having only discontinuity trickling and material in still kettle, to form residue tangible crack is arranged when the product of gathering, finished product fraction collection end is described, begin to gather after cut.
When gathering after cut part, temperature can rise slightly in the rectifying still, but it is too fast to rise, the highest 210 ℃ of can not surpass.
Equipment such as dehydration still used in the present invention, rectifying tower, rectifying still, reception still, vacuum lobe pump unit are prior art, do not repeat them here.
The present invention has following advantage:
1. by adopting the present invention, can shorten to 45 hours by 60 hours the production cycle of every still on, have technology now and shortened for 1/4th production times, thereby saved every energy consumption, reduced production cost, reduced the discharging of waste gas, waste water.
2. the tolyltriazole product appearance of existing explained hereafter be grey to Dark grey, purity is less than 90%, moisture content is less than 0.3%, ash is less than 0.05%, fusing point is 74-80 ℃; And the product appearance of producing behind employing the present invention is white, and purity is greater than 99.7%, and moisture content is less than 0.05%, and ash is less than 0.03%, and fusing point is 78-85 ℃, and visible quality product is enhanced.
3, product yield is brought up to more than 98% from existing 82%.
Description of drawings
Fig. 1 is a process flow diagram of the present invention
Among Fig. 1,1 for after cut receives still, 2 for foreshot receives still, 3 for the finished product fraction receives still, the 4th, rectifying still, the 5th, vacuum lobe pump unit, the 6th, dehydration still, the 7th, vacuum pump, the 8th, sparger, the 9th, condenser, the 10th, condensation well, the 11st, vacuum equilibration tube, the 12nd, materail tube; Rectifying still 4, sparger 8, condenser 9, condensation well 10 common formation rectifying tower.
Embodiment
Below tolyltriazole rectification process of the present invention is further described.
The present invention mainly divides two stages:
Fs: the preparation before the rectifying, i.e. dehydration.
With in the tolyltriazole production process and the intermediate oil phase material after the operation with in the vacuum suction dehydration still, close feed valve, open stirring arm, in temperature in the kettle＜150 ℃, still chuck vapor pressure is 4--6Kg/cm
2The steam heating condition under carry out normal pressure and dewatered about 3-4 hours, when temperature of charge in the still rises to 110 ℃, opening water-ring pump reduces pressure, under-0.08 to-0.09MPa pressure condition, carry out the negative pressure dehydration, when observing by looking tube that the negative pressure dehydration finishes when having a small amount of tolyltriazole to invest visor.After dehydration finishes, stop to stir the water-ring pump of closing the door, fs end-of-job.
Subordinate phase: purification rectifying.
At first open high vacuum lobe pump unit rectifying tower is vacuumized,, start the hot water oil pump, open valve rectifying tower is at the uniform velocity heated up when rectifying tower vacuum index during less than 100Pa.When the rectifying still jacket temperature rises to more than 160 ℃, should progressively turn down the deep fat fuel charging valve, slow down heat-up rate, make temperature in the kettle and jacket temperature keep≤40 ℃ the temperature difference, look running condition and regulate the fuel charging valve valve, make the temperature in the kettle rising that remains a constant speed.
When the rectifying temperature in the kettle rises to 170-180 ℃, when the rectifying tower temperature rises to 120-130 ℃, observe when backflow is arranged from the tower visor, regulate the backflow setter, make it to reflux and reach 0.5-1 hour, (if material be red-brown or goldenrod etc. than dark colour, the return time of can suitably postponing), fraction receives the still temperature and should be controlled at≤110 ℃.Be converted to when light yellow by red-brown or yellow when observing liquid material, reflux and finish, regulate the backflow setter, receive the foreshot product.During to white, begin to gather the finished product fraction by light yellow when observing the fraction color.
When normal collection finished product heated up in a steamer, the rectifying tower vacuum should be less than 100Pa, and the tower temperature is between 125-135 ℃, and should make the temperature of constant temperature water tank remain between 92-98 ℃ this moment.
When gathering finished product, should control the interior temperature of charge of rectifying still between 175-198 ℃, the rectifying tower vacuum is less than 100Pa, should regulate the cooling water valve that receives on the still simultaneously, the temperature that finished product is received in the still remains on 90-110 ℃, it is unsuitable too high to make finished product receive temperature in the kettle, guarantees effectively normal the reception.
When gathering finished product, looking when observing fraction in the tube and having only discontinuity trickling and material in still kettle, to form residue tangible crack is arranged when the product of gathering, illustrate that the finished product fraction finishes, according to this situation collection after cut.
When gathering red comprehensive look after cut part, temperature can rise slightly in the rectifying still, but it is too fast to rise, the highest 210 ℃ of can not surpass.
Whether after cut should decide rectifying to finish according to the tower temperature when gathering, and when the tower temperature drops to 90 ℃ of left and right sides naturally, shows that rectifying finishes, and closes the heating valve this moment and begins cooling.
After the collection of finished product fraction finished, the beginning blowing must the limit during blowing be put into pallet, the limit is stirred to finished product and solidifies.The purpose that stirs is to shorten the finished product solidified time, and the finished product of spontaneous curing is soft, is not easy to process other specification, and causing consuming increases.
Claims (10)
1, the rectificating method of tolyltriazole, it is characterized in that the oil phase intermediate of gained in the tolyltriazole production process and after the operation is placed in the dehydration still, in heating, go down except that the moisture content in the oil phase intermediate at normal pressure and negative pressure respectively, then dehydrated material is carried out rectifying, gather the finished product fraction according to the boiling point of tolyltriazole under the condition of heating negative pressure, obtain the tolyltriazole finished product of rectifying.
2, the rectificating method of tolyltriazole as claimed in claim 1, it is characterized in that normal pressure dehydration be in temperature in the kettle＜150 ℃, still chuck vapor pressure is 4-6Kg/cm
2The steam heating condition under carry out, dewatering is 3-4 hour.
3, the rectificating method of tolyltriazole as claimed in claim 1, it is characterized in that when temperature of charge rises to 110 ℃ in the dehydration still, begin to carry out the negative pressure dehydration, the pressure in negative pressure when dehydration should≤-0.095MPa, when observing by looking tube that the negative pressure dehydration finishes when having a small amount of tolyltriazole to invest visor.
4, the rectificating method of tolyltriazole as claimed in claim 1, after it is characterized in that dehydration finishes, under the condition of rectifying still vacuum index less than 100Pa, make that temperature at the uniform velocity heats up in the rectifying still, when the rectifying temperature in the kettle rises to 170-180 ℃, when the rectifying tower temperature rises to 120-130 ℃, make the interior feed back of still 0.5-1 hour, when liquid material in the still is converted to when light yellow by red-brown or yellow, reflux and finish, receive foreshot; When the fraction color by light yellow to when white, begin to gather the finished product fraction; The collection of finished product fraction is gathered after cut after finishing again.
5, the rectificating method of tolyltriazole as claimed in claim 4 is characterized in that should slowing down heat-up rate when the rectifying still jacket temperature rises to more than 160 ℃, makes temperature in the kettle and jacket temperature keep≤40 ℃ the temperature difference.
6, the rectificating method of tolyltriazole as claimed in claim 4, it is characterized in that the finished product fraction receive the still temperature and should be controlled at≤110 ℃.
7, the rectificating method of tolyltriazole as claimed in claim 4 is characterized in that the rectifying tower vacuum should be less than 100Pa when the collection finished product heats up in a steamer, and the tower temperature is between 125-135 ℃, and should make the temperature of constant temperature water tank remain between 92-98 ℃ this moment.
8, the rectificating method of tolyltriazole as claimed in claim 4, it is characterized in that when the collection finished product heats up in a steamer, should control the interior temperature of charge of rectifying still between 175-198 ℃, the rectifying tower vacuum is less than 100Pa, and the temperature that the finished product fraction receives in the still remains on 90-110 ℃.
9, the rectificating method of tolyltriazole as claimed in claim 4, it is characterized in that when the collection finished product heats up in a steamer, when the product of gathering is being looked when observing fraction in the tube and having only discontinuity trickling and material to form residue in still kettle tangible crack is arranged, illustrate that the collection of finished product fraction finishes, and begins to gather after cut.
10, the rectificating method of tolyltriazole as claimed in claim 4, when it is characterized in that gathering after cut, temperature can rise slightly in the rectifying still, but it is too fast to rise, the highest can not be above 210 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100388915A CN100497319C (en) | 2006-03-16 | 2006-03-16 | Rectifying method for methyl benzotrizole |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100388915A CN100497319C (en) | 2006-03-16 | 2006-03-16 | Rectifying method for methyl benzotrizole |
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| Publication Number | Publication Date |
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| CN1821232A CN1821232A (en) | 2006-08-23 |
| CN100497319C true CN100497319C (en) | 2009-06-10 |
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| CNB2006100388915A Expired - Fee Related CN100497319C (en) | 2006-03-16 | 2006-03-16 | Rectifying method for methyl benzotrizole |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102775362B (en) * | 2012-07-18 | 2013-07-10 | 如皋市金陵化工有限公司 | Cooling crystallization method of H-benzotriazole |
| US9242942B2 (en) | 2013-07-01 | 2016-01-26 | Randolph K Belter | Purification of aryltriazoles |
| CN103613554B (en) * | 2013-11-20 | 2016-06-22 | 南通波涛化工有限公司 | The continuous washing extracting system of a kind of BTA/methyl benzotriazazole and technique thereof |
| CN109836388A (en) * | 2018-12-25 | 2019-06-04 | 南通波涛化工有限公司 | A method of improving methylbenzotriazole product pH value |
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2006
- 2006-03-16 CN CNB2006100388915A patent/CN100497319C/en not_active Expired - Fee Related
Non-Patent Citations (7)
| Title |
|---|
| 《甲基苯骈三氮唑新工艺》. 王雪彦等.河北化工，第6期. 2005 |
| 《甲基苯骈三氮唑新工艺》. 王雪彦等.河北化工，第6期. 2005 * |
| 包伟.河北化工，第2005年第6期. 2005 |
| 叶红 |
| 李林 |
| 甲基苯骈三氮唑新工艺. 王雪彦 |
| 甲基苯骈三氮唑新工艺. 王雪彦；叶红；李林；包伟.河北化工，第2005年第6期. 2005 * |
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| CN1821232A (en) | 2006-08-23 |
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