CN103333062A - Preparation method of m-hydroxybenzaldehyde - Google Patents
Preparation method of m-hydroxybenzaldehyde Download PDFInfo
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- CN103333062A CN103333062A CN201310280943XA CN201310280943A CN103333062A CN 103333062 A CN103333062 A CN 103333062A CN 201310280943X A CN201310280943X A CN 201310280943XA CN 201310280943 A CN201310280943 A CN 201310280943A CN 103333062 A CN103333062 A CN 103333062A
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Abstract
The invention relates to the technical field of m-hydroxybenzaldehyde, particularly to a preparation method of m-hydroxybenzaldehyde. The product is prepared by an esterification section, a chlorination section, a distillation section, a hydrolysis section, a refining section and a drying section. The raw materials and auxiliary materials of the product are easily available, the technological steps are simplified, pollutants are fewer, the product yield is up to more than 85%, the weight of the product is easy to control, and the product cost is reduced by about 20% compared with the past. The product can be used for making epinephrine and its derivatives, phenylephrine hydrochloride and the like in medicine; in the metal industry, the product can serve as a nickel plating brightener, and can be used for corrosion prevention and decoration of steel, copper and copper alloys, zinc die castings, aluminum alloys and the like; in the spice industry, the product can be directly used as a spice, or can be used for making spices after esterification, etherification and derivative reactions; and also, a small amount of the product can be used as a quantitative analysis reagent of sugar.
Description
Technical field
The present invention relates to the m-hydroxybenzaldehyde technical field, be specifically related to the preparation method of m-hydroxybenzaldehyde.
Background technology
M-hydroxybenzaldehyde is a kind of purposes fine chemical product very widely, can be widely used in production industries such as medicine, dyestuff, sterilant, spices, photograph emulsifying agent.But its complex manufacturing of the m-hydroxybenzaldehyde of prior art, production cost be big, it is serious to stain, be difficult for accomplishing to clean production, and quality product is also wayward simultaneously.
Summary of the invention
The purpose of this invention is to provide the preparation method that a kind of production technique is simple, stain less, clean production, the manageable m-hydroxybenzaldehyde of quality product.
In order to solve the existing problem of background technology, the present invention is by the following technical solutions: the preparation method of m-hydroxybenzaldehyde, comprise esterification workshop section, chlorination workshop section, distillation workshop section, hydrolysis workshop section, refining workshop section and dry workshop section, and concrete steps are as follows:
(1), esterification workshop section
By weight meta-cresol 400～600kg, diacetyl oxide 460～500kg are put in the 2000L glassed steel reaction vessels by the header tank metering, slowly heat up, kettle temperature begins insulation when reaching 130 ℃, be incubated 4～5 hours, and temperature is controlled at 130 ℃～140 ℃; Carry out air distillation after insulation finishes and collect by-product acetic acid, acetic acid is analyzed warehousing after passing; To open then and cool to 90 ℃～100 ℃, be extracted into thick ester in the esterification still pot to be distilled, open oil-sealed rotary pump, close the emptying valve, make whole Distallation systm be in vacuum state, open and take out the material valve, in thick ester suction still pot, open the low valve that boils, close the valve that just boils, open jacket steam and heat up, make it steam low-boiling-point substance, when tower top temperature reaches 135 ℃～145 ℃, vacuum pressure 0.092～0.095Mpa, close the low valve that boils, receive before the back of just boiling 150Kg and be defective ester and return still pot and steam altogether with following batch, after be qualified ester collection;
(2), chlorination workshop section
By weight with trichloromethane 600～800kg, above-mentioned qualified ester, methylene dichloride 380～400kg, urotropine 900～1000kg, Diisopropyl azodicarboxylate 180～220kg puts in the 3000L glassed steel reaction vessels, open the reactor jacket steam, slowly heat up, when the temperature indication reaches 55 ℃～60 ℃, open logical chlorine valve door and cock and begin logical chlorine, logical chlorine dose steel cylinder compensator or trimmer pressure is 0.05～0.1Mpa during beginning, the control in first hour of logical chlorine is at 7～13Kg per hour, logical chlorine speed visual response phenomenon is regulated, per hour control at 15～21Kg after spending 1 hour, the logical chlorine speed control that slowed down in two hours that draws to an end when logical chlorine dose is at 7～13Kg per hour, in logical chlorine process, should keep a close eye on temperature regime simultaneously, temperature of reaction should be controlled to be 65 ℃～75 ℃, logical chlorine finishes insulation 15 minutes, cuts off light source, opens the chuck water coolant, make it be cooled to close all valves below 50 ℃;
(3), distillation workshop section
The muriate of chlorine of will having friendly relations is drawn into still pot, and it is mouthful airtight good to take out material after exhausting, and has prevented that moisture content from advancing in the still pot; Open the vacuum unit, recorded the liquid level numerical index of trichloromethane storage vessel, open jacket steam and slowly heat up by it; Vacuum tightness remains 0.03～0.07Mpa, and distillation temperature is controlled to be 50 ℃～90 ℃, and end temp should be controlled below 100 ℃, distillation finishes, open water coolant, make it be cooled to the suction filtration of back below 50 ℃ and advance hydrolysis in the hydrolyzer, filter cake concentrates separately and reclaims the by-product hydrochloric acid urotropine;
(4), hydrolysis workshop section
Again calcium carbonate 300～500kg, tap water 400～600kg are put in the hydrolyzer by weight, open the intensification of jacket steam valve and normally open stirring, when temperature in 70 ℃～80 ℃, heat-up rate should slow down as far as possible, when temperature reaches 100 ℃～102 ℃ of processing requirements, in visor, there is backflow phenomenon to get final product, heating up begins insulation when reaching 100 ℃, being incubated after 30 hours is the hydrolysis terminal point, carries out suction filtration immediately; Before carrying out suction filtration, start tool vacuum pump and valve with suction filtration bucket and pipeline preheating, carry out normal suction filtration with 80 ℃ of hot water then, and suction filtration finishes and closes mechanical pump and valve; Open crystallizing pan and stir, open the chuck water coolant, make its naturally cooling, when temperature is as cold as room temperature, close water coolant, open freezing fluid valve, when temperature is 10 ℃～15 ℃, can get rid of filter, carry out then packed, weigh and carry out the crude product record, close refrigerator;
(5), refining workshop section
M-hydroxybenzaldehyde crude product, activated carbon, water are put in the reactor, open the logical steam of stirring reaction pot chuck, it is slowly heated up, temperature control kept 15 minutes in this temperature province at 60 ℃～75 ℃, stop again stirring, open oil-sealed rotary pump and valve and carry out hot suction filtration, get rid of filter then, filter cake carries out the dried recovered product, and filtrate is advanced wastewater treatment;
(6), dry workshop section
With the m-hydroxybenzaldehyde that gets rid of the barrelling of the filter back laggard baking oven that sieves, oven temperature is 60 ℃～75 ℃, dry by the fire 6 hours post analysis and packs and carry out the metering record.
Wherein, main chemical equation is as follows:
The present invention has following beneficial effect: the preparation method of m-hydroxybenzaldehyde of the present invention, make product through esterification workshop section, chlorination workshop section, distillation workshop section, hydrolysis workshop section, refining workshop section and dry workshop section, its products material, auxiliary material simply are simple and easy to, processing step is simplified, pollutent is few, product yield is up to more than 85%, product weight is stable control easily, product cost is compared than before and is reduced about 20%, its product is pharmaceutically in order to make the disorderly and derivative of suprarenal gland, m-Sympatol etc.; Be used as nickel plating brightener, corrosion protection and the decoration of iron and steel, copper and copper alloy, zine pressure casting, aluminium alloy etc. in metal industry; Can directly be used as spices in fragrance industry, or be used further to make spices through esterification, etherificate and derivatization reaction; Also can be used as the quantitative analysis reagent of carbohydrate on a small quantity.In addition, production technique of the present invention is simple, production unit is advanced, easy to operate, production cost is low, realize minimize contamination.
Embodiment
Below the present invention will be further described in detail.
Embodiment one:
The preparation method of m-hydroxybenzaldehyde comprises esterification workshop section, chlorination workshop section, distillation workshop section, hydrolysis workshop section, refining workshop section and dry workshop section, and concrete steps are as follows:
(1), esterification workshop section
By weight meta-cresol 400kg, diacetyl oxide 460kg are put in the 2000L glassed steel reaction vessels by the header tank metering, slowly heat up, kettle temperature begins insulation when reaching 130 ℃, be incubated 4 hours, and temperature is controlled at 130 ℃; Carry out air distillation after insulation finishes and collect by-product acetic acid, acetic acid is analyzed warehousing after passing; To open then and cool to 90 ℃, be extracted into thick ester in the esterification still pot to be distilled, open oil-sealed rotary pump, close the emptying valve, make whole Distallation systm be in vacuum state, open and take out the material valve, in thick ester suction still pot, open the low valve that boils, close the valve that just boils, open jacket steam and heat up, make it steam low-boiling-point substance, when tower top temperature reaches 135 ℃, vacuum pressure 0.092Mpa, close the low valve that boils, receive before the back of just boiling 150Kg and be defective ester and return still pot and steam altogether with following batch, after be qualified ester collection.
(2), chlorination workshop section
By weight with trichloromethane 600kg, above-mentioned qualified ester, methylene dichloride 380kg, urotropine 900kg, Diisopropyl azodicarboxylate 180kg puts in the 3000L glassed steel reaction vessels, open the reactor jacket steam, slowly heat up, when the temperature indication reaches 55 ℃, open logical chlorine valve door and cock and begin logical chlorine, logical chlorine dose steel cylinder compensator or trimmer pressure is 0.05Mpa during beginning, the control in first hour of logical chlorine is at 7Kg per hour, logical chlorine speed visual response phenomenon is regulated, per hour control at 15Kg after spending 1 hour, the logical chlorine speed control that draw to an end when logical chlorine dose two hours slows down should be kept a close eye on temperature regime simultaneously at 7Kg per hour in logical chlorine process, temperature of reaction should be controlled to be 65 ℃, logical chlorine finishes insulation 15 minutes, cuts off light source, opens the chuck water coolant, make it be cooled to close all valves below 50 ℃.
(3), distillation workshop section
The muriate of chlorine of will having friendly relations is drawn into still pot, and it is mouthful airtight good to take out material after exhausting, and has prevented that moisture content from advancing in the still pot; Open the vacuum unit, recorded the liquid level numerical index of trichloromethane storage vessel, open jacket steam and slowly heat up by it; Vacuum tightness remains 0.03Mpa, and distillation temperature is controlled to be 50 ℃, and end temp should be controlled below 100 ℃, and distillation finishes, and opens water coolant, makes it be cooled to the suction filtration of back below 50 ℃ and advances hydrolysis in the hydrolyzer, and filter cake concentrates separately and reclaims the by-product hydrochloric acid urotropine.
(4), hydrolysis workshop section
Again calcium carbonate 300kg, tap water 400kg are put in the hydrolyzer by weight, open the intensification of jacket steam valve and normally open stirring, when temperature in 70 ℃, heat-up rate should slow down as far as possible, when temperature reaches 100 ℃ of processing requirements, in visor, there is backflow phenomenon to get final product, heating up begins insulation when reaching 100 ℃, being incubated after 30 hours is the hydrolysis terminal point, carries out suction filtration immediately; Before carrying out suction filtration, start tool vacuum pump and valve with suction filtration bucket and pipeline preheating, carry out normal suction filtration with 80 ℃ of hot water then, and suction filtration finishes and closes mechanical pump and valve; Open crystallizing pan and stir, open the chuck water coolant, make its naturally cooling, when temperature is as cold as room temperature, close water coolant, open freezing fluid valve, when temperature is 10 ℃, can get rid of filter, carry out then packed, weigh and carry out the crude product record, close refrigerator.
(5), refining workshop section
M-hydroxybenzaldehyde crude product, activated carbon, water are put in the reactor, open the logical steam of stirring reaction pot chuck, it is slowly heated up, temperature control kept 15 minutes in the time of 60 ℃, stop again stirring, open oil-sealed rotary pump and valve and carry out hot suction filtration, need to prove, before suction filtration, should be earlier with about 80 ℃ hot water suction filtration utensil and pipeline be carried out preheating; Kettle temperature is opened the chilled brine cooling after reaching room temperature, when temperature is cooled to 15 ℃ of left and right sides blowings; Blowing gets rid of filter after finishing, and filter cake carries out the dried recovered product, and filtrate is advanced wastewater treatment.
(6), dry workshop section
With the m-hydroxybenzaldehyde that gets rid of the barrelling of the filter back laggard baking oven that sieves, oven temperature is 60 ℃, dry by the fire 6 hours post analysis and packs and carry out the metering record.
In the present embodiment, esterification has acetic acid to generate, and distillation is reclaimed and done by-product, has non-condensable gas to produce; Chlorination reaction has hydrogen chloride gas to produce, for urotropine is tied up sour salify; Hydrolysis reaction generates hydrogenchloride, methyl alcohol produces, and methanol condensed reclaims and does by-product, and hydrogenchloride and calcium carbonate reaction are produced the calcium chloride recovery and done by-product; Organic solvent has a small amount of volatilization waste gas to produce when feeding in raw material, distillation is reclaimed the non-condensable gas generation, and the hc effluent warp concentrates to wait and reclaims the processing of the laggard waste water processing station of by-product salt, handles outside distillation slag is all entrusted.
Embodiment two:
The preparation method of m-hydroxybenzaldehyde comprises esterification workshop section, chlorination workshop section, distillation workshop section, hydrolysis workshop section, refining workshop section and dry workshop section, and concrete steps are as follows:
(1), esterification workshop section
By weight meta-cresol 500kg, diacetyl oxide 480kg are put in the 2000L glassed steel reaction vessels by the header tank metering, slowly heat up, kettle temperature begins insulation when reaching 130 ℃, be incubated 4.5 hours, and temperature is controlled at 135 ℃; Carry out air distillation after insulation finishes and collect by-product acetic acid, acetic acid is analyzed warehousing after passing; To open then and cool to 95 ℃, be extracted into thick ester in the esterification still pot to be distilled, open oil-sealed rotary pump, close the emptying valve, make whole Distallation systm be in vacuum state, open and take out the material valve, in thick ester suction still pot, open the low valve that boils, close the valve that just boils, open jacket steam and heat up, make it steam low-boiling-point substance, when tower top temperature reaches 140 ℃, vacuum pressure 0.094Mpa, close the low valve that boils, receive before the back of just boiling 150Kg and be defective ester and return still pot and steam altogether with following batch, after be qualified ester collection.
(2), chlorination workshop section
By weight with trichloromethane 700kg, above-mentioned qualified ester, methylene dichloride 390kg, urotropine 950kg, Diisopropyl azodicarboxylate 200kg puts in the 3000L glassed steel reaction vessels, open the reactor jacket steam, slowly heat up, when the temperature indication reaches 58 ℃, open logical chlorine valve door and cock and begin logical chlorine, logical chlorine dose steel cylinder compensator or trimmer pressure is 0.08Mpa during beginning, the control in first hour of logical chlorine is at 10Kg per hour, logical chlorine speed visual response phenomenon is regulated, per hour control at 18Kg after spending 1 hour, the logical chlorine speed control that draw to an end when logical chlorine dose two hours slows down should be kept a close eye on temperature regime simultaneously at 10Kg per hour in logical chlorine process, temperature of reaction should be controlled to be 70 ℃, logical chlorine finishes insulation 15 minutes, cuts off light source, opens the chuck water coolant, make it be cooled to close all valves below 50 ℃.
(3), distillation workshop section
The muriate of chlorine of will having friendly relations is drawn into still pot, and it is mouthful airtight good to take out material after exhausting, and has prevented that moisture content from advancing in the still pot; Open the vacuum unit, recorded the liquid level numerical index of trichloromethane storage vessel, open jacket steam and slowly heat up by it; Vacuum tightness remains 0.05Mpa, and distillation temperature is controlled to be 70 ℃, and end temp should be controlled below 100 ℃, and distillation finishes, and opens water coolant, makes it be cooled to the suction filtration of back below 50 ℃ and advances hydrolysis in the hydrolyzer, and filter cake concentrates separately and reclaims the by-product hydrochloric acid urotropine.
(4), hydrolysis workshop section
Again calcium carbonate 400kg, tap water 500kg are put in the hydrolyzer by weight, open the intensification of jacket steam valve and normally open stirring, when temperature in 75 ℃, heat-up rate should slow down as far as possible, when temperature reaches 101 ℃ of processing requirements, in visor, there is backflow phenomenon to get final product, heating up begins insulation when reaching 100 ℃, being incubated after 30 hours is the hydrolysis terminal point, carries out suction filtration immediately; Before carrying out suction filtration, start tool vacuum pump and valve with suction filtration bucket and pipeline preheating, carry out normal suction filtration with 80 ℃ of hot water then, and suction filtration finishes and closes mechanical pump and valve; Open crystallizing pan and stir, open the chuck water coolant, make its naturally cooling, when temperature is as cold as room temperature, close water coolant, open freezing fluid valve, when temperature is 12 ℃, can get rid of filter, carry out then packed, weigh and carry out the crude product record, close refrigerator.
(5), refining workshop section
M-hydroxybenzaldehyde crude product, activated carbon, water are put in the reactor, open the logical steam of stirring reaction pot chuck, it is slowly heated up, temperature control 70 ℃ the time kept 15 minutes, stop again stirring, open oil-sealed rotary pump and valve and carry out hot suction filtration, get rid of filter then, filter cake carries out the dried recovered product, and filtrate is advanced wastewater treatment.
(6), dry workshop section
With the m-hydroxybenzaldehyde that gets rid of the barrelling of the filter back laggard baking oven that sieves, oven temperature is 68 ℃, dry by the fire 6 hours post analysis and packs and carry out the metering record.
Embodiment three:
The preparation method of m-hydroxybenzaldehyde comprises esterification workshop section, chlorination workshop section, distillation workshop section, hydrolysis workshop section, refining workshop section and dry workshop section, and concrete steps are as follows:
(1), esterification workshop section
By weight meta-cresol 600kg, diacetyl oxide 500kg are put in the 2000L glassed steel reaction vessels by the header tank metering, slowly heat up, kettle temperature begins insulation when reaching 130 ℃, be incubated 5 hours, and temperature is controlled at 140 ℃; Carry out air distillation after insulation finishes and collect by-product acetic acid, acetic acid is analyzed warehousing after passing; To open then and cool to 100 ℃, be extracted into thick ester in the esterification still pot to be distilled, open oil-sealed rotary pump, close the emptying valve, make whole Distallation systm be in vacuum state, open and take out the material valve, in thick ester suction still pot, open the low valve that boils, close the valve that just boils, open jacket steam and heat up, make it steam low-boiling-point substance, when tower top temperature reaches 145 ℃, vacuum pressure 0.095Mpa, close the low valve that boils, receive before the back of just boiling 150Kg and be defective ester and return still pot and steam altogether with following batch, after be qualified ester collection.
(2), chlorination workshop section
By weight with trichloromethane 800kg, above-mentioned qualified ester, methylene dichloride 400kg, urotropine 1000kg, Diisopropyl azodicarboxylate 220kg puts in the 3000L glassed steel reaction vessels, open the reactor jacket steam, slowly heat up, when the temperature indication reaches 60 ℃, open logical chlorine valve door and cock and begin logical chlorine, logical chlorine dose steel cylinder compensator or trimmer pressure is 0.1Mpa during beginning, the control in first hour of logical chlorine is at 13Kg per hour, logical chlorine speed visual response phenomenon is regulated, per hour control at 21Kg after spending 1 hour, the logical chlorine speed control that draw to an end when logical chlorine dose two hours slows down should be kept a close eye on temperature regime simultaneously at 13Kg per hour in logical chlorine process, temperature of reaction should be controlled to be 75 ℃, logical chlorine finishes insulation 15 minutes, cuts off light source, opens the chuck water coolant, make it be cooled to close all valves below 50 ℃.
(3), distillation workshop section
The muriate of chlorine of will having friendly relations is drawn into still pot, and it is mouthful airtight good to take out material after exhausting, and has prevented that moisture content from advancing in the still pot; Open the vacuum unit, recorded the liquid level numerical index of trichloromethane storage vessel, open jacket steam and slowly heat up by it; Vacuum tightness remains 0.07Mpa, and distillation temperature is controlled to be 90 ℃, and end temp should be controlled below 100 ℃, and distillation finishes, and opens water coolant, makes it be cooled to the suction filtration of back below 50 ℃ and advances hydrolysis in the hydrolyzer, and filter cake concentrates separately and reclaims the by-product hydrochloric acid urotropine.
(4), hydrolysis workshop section
Again calcium carbonate 500kg, tap water 600kg are put in the hydrolyzer by weight, open the intensification of jacket steam valve and normally open stirring, when temperature during at 80 ℃, heat-up rate should slow down as far as possible, when temperature reaches 102 ℃ of processing requirements, in visor, there is backflow phenomenon to get final product, heating up begins insulation when reaching 100 ℃, being incubated after 30 hours is the hydrolysis terminal point, carries out suction filtration immediately; Before carrying out suction filtration, start tool vacuum pump and valve with suction filtration bucket and pipeline preheating, carry out normal suction filtration with 80 ℃ of hot water then, and suction filtration finishes and closes mechanical pump and valve; Open crystallizing pan and stir, open the chuck water coolant, make its naturally cooling, when temperature is as cold as room temperature, close water coolant, open freezing fluid valve, when temperature is 15 ℃, can get rid of filter, carry out then packed, weigh and carry out the crude product record, close refrigerator.
(5), refining workshop section
M-hydroxybenzaldehyde crude product, activated carbon, water are put in the reactor, open the logical steam of stirring reaction pot chuck, it is slowly heated up, temperature control kept 15 minutes in the time of 75 ℃, stop again stirring, open oil-sealed rotary pump and valve and carry out hot suction filtration, get rid of filter then, filter cake carries out the dried recovered product, and filtrate is advanced wastewater treatment.
(6), dry workshop section
With the m-hydroxybenzaldehyde that gets rid of the barrelling of the filter back laggard baking oven that sieves, oven temperature is 75 ℃, dry by the fire 6 hours post analysis and packs and carry out the metering record.
Explanation is at last, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, other modifications that those of ordinary skills make technical scheme of the present invention or be equal to replacement, only otherwise break away from the spirit and scope of technical solution of the present invention, all should be encompassed in the middle of the claim scope of the present invention.
Claims (1)
1. the preparation method of m-hydroxybenzaldehyde is characterized in that, comprises esterification workshop section, chlorination workshop section, distillation workshop section, hydrolysis workshop section, refining workshop section and dry workshop section, and concrete steps are as follows:
(1), esterification workshop section
By weight meta-cresol 400～600kg, diacetyl oxide 460～500kg are put in the 2000L glassed steel reaction vessels by the header tank metering, slowly heat up, kettle temperature begins insulation when reaching 130 ℃, be incubated 4～5 hours, and temperature is controlled at 130 ℃～140 ℃; Carry out air distillation after insulation finishes and collect by-product acetic acid, acetic acid is analyzed warehousing after passing; To open then and cool to 90 ℃～100 ℃, be extracted into thick ester in the esterification still pot to be distilled, open oil-sealed rotary pump, close the emptying valve, make whole Distallation systm be in vacuum state, open and take out the material valve, in thick ester suction still pot, open the low valve that boils, close the valve that just boils, open jacket steam and heat up, make it steam low-boiling-point substance, when tower top temperature reaches 135 ℃～145 ℃, vacuum pressure 0.092～0.095Mpa, close the low valve that boils, receive before the back of just boiling 150Kg and be defective ester and return still pot and steam altogether with following batch, after be qualified ester collection;
(2), chlorination workshop section
By weight with trichloromethane 600～800kg, above-mentioned qualified ester, methylene dichloride 380～400kg, urotropine 900～1000kg, Diisopropyl azodicarboxylate 180～220kg puts in the 3000L glassed steel reaction vessels, open the reactor jacket steam, slowly heat up, when the temperature indication reaches 55 ℃～60 ℃, open logical chlorine valve door and cock and begin logical chlorine, logical chlorine dose steel cylinder compensator or trimmer pressure is 0.05～0.1Mpa during beginning, the control in first hour of logical chlorine is at 7～13Kg per hour, logical chlorine speed visual response phenomenon is regulated, per hour control at 15～21Kg after spending 1 hour, the logical chlorine speed control that slowed down in two hours that draws to an end when logical chlorine dose is at 7～13Kg per hour, in logical chlorine process, should keep a close eye on temperature regime simultaneously, temperature of reaction should be controlled to be 65 ℃～75 ℃, logical chlorine finishes insulation 15 minutes, cuts off light source, opens the chuck water coolant, make it be cooled to close all valves below 50 ℃;
(3), distillation workshop section
The muriate of chlorine of will having friendly relations is drawn into still pot, and it is mouthful airtight good to take out material after exhausting, and has prevented that moisture content from advancing in the still pot; Open the vacuum unit, recorded the liquid level numerical index of trichloromethane storage vessel, open jacket steam and slowly heat up by it; Vacuum tightness remains 0.03～0.07Mpa, and distillation temperature is controlled to be 50 ℃～90 ℃, and end temp should be controlled below 100 ℃, distillation finishes, open water coolant, make it be cooled to the suction filtration of back below 50 ℃ and advance hydrolysis in the hydrolyzer, filter cake concentrates separately and reclaims the by-product hydrochloric acid urotropine;
(4), hydrolysis workshop section
Again calcium carbonate 300～500kg, tap water 400～600kg are put in the hydrolyzer by weight, open the intensification of jacket steam valve and normally open stirring, when temperature in 70 ℃～80 ℃, heat-up rate should slow down as far as possible, when temperature reaches 100 ℃～102 ℃ of processing requirements, in visor, there is backflow phenomenon to get final product, heating up begins insulation when reaching 100 ℃, being incubated after 30 hours is the hydrolysis terminal point, carries out suction filtration immediately; Before carrying out suction filtration, start tool vacuum pump and valve with suction filtration bucket and pipeline preheating, carry out normal suction filtration with 80 ℃ of hot water then, and suction filtration finishes and closes mechanical pump and valve; Open crystallizing pan and stir, open the chuck water coolant, make its naturally cooling, when temperature is as cold as room temperature, close water coolant, open freezing fluid valve, when temperature is 10 ℃～15 ℃, can get rid of filter, carry out then packed, weigh and carry out the crude product record, close refrigerator;
(5), refining workshop section
M-hydroxybenzaldehyde crude product, activated carbon, water are put in the reactor, open the logical steam of stirring reaction pot chuck, it is slowly heated up, temperature control kept 15 minutes in this temperature province at 60 ℃～75 ℃, stop again stirring, open oil-sealed rotary pump and valve and carry out hot suction filtration, get rid of filter then, filter cake carries out the dried recovered product, and filtrate is advanced wastewater treatment;
(6), dry workshop section
With the m-hydroxybenzaldehyde that gets rid of the barrelling of the filter back laggard baking oven that sieves, oven temperature is 60 ℃～75 ℃, dry by the fire 6 hours post analysis and packs and carry out the metering record.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109053443A (en) * | 2018-08-06 | 2018-12-21 | 杭州华东医药集团浙江华义制药有限公司 | The bromo- 3- aldehyde radical-phenoxy group of 4-(4-)-benzonitrile synthetic method |
| CN111302911A (en) * | 2020-03-18 | 2020-06-19 | 潍坊润谱化学有限公司 | Preparation method of m-hydroxybenzaldehyde |
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| JPS62155236A (en) * | 1985-12-27 | 1987-07-10 | Seitetsu Kagaku Co Ltd | Production of hydroxybenzaldehyde |
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| JPS62155236A (en) * | 1985-12-27 | 1987-07-10 | Seitetsu Kagaku Co Ltd | Production of hydroxybenzaldehyde |
Non-Patent Citations (1)
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| 姜一飞等: "间羟基苯甲醛的合成路线述评", 《浙江化工》, vol. 27, no. 2, 31 December 1996 (1996-12-31), pages 12 - 15 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109053443A (en) * | 2018-08-06 | 2018-12-21 | 杭州华东医药集团浙江华义制药有限公司 | The bromo- 3- aldehyde radical-phenoxy group of 4-(4-)-benzonitrile synthetic method |
| CN111302911A (en) * | 2020-03-18 | 2020-06-19 | 潍坊润谱化学有限公司 | Preparation method of m-hydroxybenzaldehyde |
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