CN1099430C - Process and special equipment for polymerizing polymethanopolyphenyl polyisocyanate - Google Patents

Process and special equipment for polymerizing polymethanopolyphenyl polyisocyanate Download PDF

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Publication number
CN1099430C
CN1099430C CN98110586A CN98110586A CN1099430C CN 1099430 C CN1099430 C CN 1099430C CN 98110586 A CN98110586 A CN 98110586A CN 98110586 A CN98110586 A CN 98110586A CN 1099430 C CN1099430 C CN 1099430C
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poly
flavor
polymerization
isocyanate
production method
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CN1254724A (en
Inventor
申运栓
孙敦孝
杨万宏
丁建生
卫剑峰
姜英明
王青海
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Wanhua Chemical Group Co Ltd
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Yantai Wanhua Polyurethanes Co Ltd
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Abstract

The present invention discloses a method and a special device for producing polymerized polymethene polyphenyl polyisocyanate, which belongs to the technical field of preparation of high molecular compounds. The present invention has the technical scheme that purification processing technology to primary distillate is added on the basis of the existing producing method; the primary distillate is heated to 120 DEG C to 220 DEG C; inert gas is filled into a deodorizing pot to be dispersed and deodoured under the conditions that the vacuum pressure in the deodorizing pot is between 0 and 300 mmHg, the time is between 10 and 200 minutes; subsequently, the primary distillate is cooled to 40 DEG C to 60 DEG C; the special device is the sealed deodorizing pot which is a cavity, and at least three dispersing tubes which are uniformly distributed at an angle of 360 DEG in the layered staggering structure are arranged in the cavity. The present invention which has the advantages of small treating capacity, simplicity, convenience and low expense reduces the environmental pollution and the encroachment to the health of human bodies.

Description

A kind of production method of polymerization poly methylene poly phenyl poly isocyanate and isolated plant
The present invention relates to the organic high molecular compound preparing technical field, relate in particular to a kind of production method and specific equipment of polymerization poly methylene poly phenyl poly isocyanate.
The polymerization poly methylene poly phenyl poly isocyanate is the main raw material of urethane industry, with mixed foamings such as it and polyether glycol, catalyzer, whipping agents and the soft bubble rosin products of various rigid polyurethanes that makes, be widely used in all trades and professions, for industrial production with satisfy the growing culture of people and living needs has been brought into play positive effect.Yet because the light constituent impurity that produces in the polymerization poly methylene poly phenyl poly isocyanate production process can not be got rid of totally effectively, remain in the polymerization poly methylene poly phenyl poly isocyanate product, cause in the foaming process because the effect and the chemical action of heat, impurity is discharged in the air, produce the strong impulse smell, stimulate human respiratory, eyes are shed tears, not only influence HUMAN HEALTH, and contaminate environment.For solving this disadvantage, the patent No. of United States Patent Office (USPO) bulletin in 14 days October nineteen ninety-five is: only propose to put forward an operation with rare gas element gas under the low pressure pungent odour light constituent impurity that has of poly methylene poly phenyl poly isocyanate production process is removed putting forward removal of impurity technological process in the technical scheme of US3912600.Though this technical scheme can reach the less effect of foreign matter content, the light constituent impurity enriched that behind two step separation circuits irritating smell is arranged is in starting fraction, and its concentration is still higher.If want enrichment concentration lower, certainly will need to strengthen the effect that removes of rare gas element under the low pressure, the small amount of impurities in a large amount of thick poly methylene poly phenyl poly isocyanates is removed again, not only treatment capacity is many, and difficulty is big.
The objective of the invention is to improve the deficiency of prior art, and provide a kind of treatment capacity few, treatment process is simple and easy to do, and expense is low, and irritating smell removes the production method and the specific equipment of polymerization poly methylene poly phenyl poly isocyanate more completely.
The objective of the invention is to be achieved by following technical solution a kind of production method of polymerization poly methylene poly phenyl poly isocyanate.It comprises condensation reaction, phosgenation reaction successively, removes phosgene, removes inert solvent, proposes the removal of impurity, flash liberation.Technological process such as secondary separation, mixing, its special character are that this production method is to be provided with the purification processes technological process between secondary separation and hybrid technique process; Described purification processes technological process is that starting fraction is heated to 120-220 ℃, vacuum pressure is 0-300mmHg in taking off the flavor still, time is under 10-200 minute the condition, disperse to take off flavor by the input rare gas element and handle, be chilled to 40-60 ℃ afterwards and mix with first polymerization poly methylene poly phenyl poly isocyanate again.
For further realizing purpose of the present invention, above-mentioned purification processes technological process is that starting fraction is heated to 150-200 ℃, vacuum pressure is 0-100mmHg in taking off the flavor still, time is under 30-100 minute the condition, disperse to take off flavor by the input rare gas element and handle, be chilled to 45-50 ℃ afterwards and mix with first polymerization poly methylene poly phenyl poly isocyanate again.
For realizing purpose of the present invention, implement the isolated plant of aforementioned production method, it by well heater, condenser, water cooler etc. by pipeline with take off the flavor still institute that is connected to one and form, its special character is that this isolated plant comprises that taking off the still of distinguishing the flavor of is airtight cavity.The rare gas element input tube is fixedly connected on and takes off the bottom that flavor still upper center and extending is taken off flavor still cavity, its tube end be provided with at least three and in 360 ° of scopes uniform distribution and be the dispersion pipe that the stratiform dislocation type is provided with.
Compared with the prior art the present invention has following unusual effect: the first is because the scheme that the present invention takes is the starting fraction after the secondary separation to be disperseed to take off flavor handle, not only solve the disadvantage that treatment capacity is many, difficulty is big that prior art removes a small amount of impurity in a large amount of thick poly methylene poly phenyl poly isocyanates again, and solved unsolved for many years in the art problem; It two is because the present invention adopts rare gas element that starting fraction is taken off flavor under the condition of heating vacuum pressure handles, method is simple, it is few to handle T skill process device investment cost, the treating processes expense is low, accomplish that quality product is more excellent under the constant condition of currently available products use range, price; It three is because method of the present invention correctly is suitable for, making the hydrolyzable chloride content of handling preceding starting fraction is 0.02-0.06%, color is yellow, chromatic number is a 60-150 platinum cobalt number, the pungent hydrolyzable chloride content that becomes processing back starting fraction of smell is 0.001-0.003%, chromatic number is a 10-20 platinum cobalt number, and irritating smell does not have, and hydrolyzable chloride content and chromatic number index are better than the index request of the pure diphenylmethanediisocyanate of national standard top grade; It four is because the strong impulse smell that exists in the prior art has been eliminated in the enforcement of technical solution of the present invention, has not only eliminated health effects, and can not cause environmental pollution, helps the further expansion use range to this product.
The production method of a kind of polymerization poly methylene poly phenyl poly isocyanate of the present invention and the concrete production process of isolated plant and concrete structure are provided by the following drawings and embodiment.
Fig. 1 is a kind of production process flow process figure of polymerization poly methylene poly phenyl poly isocyanate.
Fig. 2 is a purification processes process flow diagram flow chart in a kind of production method of polymerization poly methylene poly phenyl poly isocyanate.
Fig. 3 is a kind of isolated plant structural representation of method of production polymerization poly methylene poly phenyl poly isocyanate.
Fig. 4 is the A-A sectional view of Fig. 3.
Fig. 5 is another structural representation of isolated plant of a kind of method of production polymerization poly methylene poly phenyl poly isocyanate.
Fig. 6 is the B-B sectional view of Fig. 5.
Describe the production method of a kind of polymerization poly methylene poly phenyl poly isocyanate of the present invention and the concrete production technique and the specific structural details of isolated plant in detail below in conjunction with accompanying drawing.
Embodiment 1
A kind of production method of polymerization poly methylene poly phenyl poly isocyanate (referring to accompanying drawing 1), it is the raw material (aniline with poly methylene poly phenyl poly isocyanate, water, hydrochloric acid, formaldehyde etc.) after condensation reaction 1 reaction, making thick poly methylene poly phenyl poly isocyanate under the condition of relevant devices, in the presence of inert solvent, carry out phosgenation reaction 2 and get photochemical liquid with phosgene, again through removing remaining phosgene 3 steps, remove inert solvent step 4 and get impure more thick poly methylene poly phenyl poly isocyanate, this thick poly methylene poly phenyl poly isocyanate is carried impurity 5 with rare gas element gas under low pressure mode is removed a large amount of impurity and is got impure less thick poly methylene poly phenyl poly isocyanate, carry out 6 one-tenth thick pure diphenylmethanediisocyanates of flash liberation and first polymerization poly methylene poly phenyl poly isocyanate with thin-film evaporator then, thick pure diphenylmethanediisocyanate further is separated into starting fraction through secondary separation 7, pure diphenylmethanediisocyanate and after cut; Pure diphenylmethanediisocyanate product is through product packing 9.Dispatch from the factory after the packing.After cut will mix use in proportion with first polymerization poly methylene poly phenyl poly isocyanate; The quality index of starting fraction this moment is generally: hydrolyzable chloride content is 0.02-0.06%, and color be yellow, and chromatic number is a 60-150 platinum cobalt number, and smell is pungent.Present embodiment is starting fraction to be carried out primary purification again handle 8 (referring to accompanying drawings 2), its treating processes is the intermittent type processing mode, it is that starting fraction is heated to 120-150 ℃ and take off 1000kg in the flavor still 14 by pipeline input in well heater 12, and taking off the still 14 of distinguishing the flavor of is an airtight cavity, N 2Be input in the cavity that takes off flavor still 14 and by pipeline 13 and taking off 14 diffusions of flavor still, logical N by the equally distributed dispersion pipe 15 that is in 360 ° of scopes of one deck that is provided with within it 2Amount is 10Nm 3/ h; Taking off flavor still 13 interior vacuum pressures is between the 100-200mmHg; Processing time is 100-200 minute; Open then the valve 23 on the cooler pipeline; Head fraction discharging after the processing enters cooler 21 and carries out quenching; Make it be chilled to 40-45 ℃; Enter again basin 22; Mix in proportion 10 with first polymerization poly methylene poly phenyl poly isocyanate, tails; And carry out dispatching from the factory after the packing 11; Can produce the product that polymerization poly methylene poly phenyl poly isocyanate of the present invention has no irritating odor
The isolated plant of the method for production polymerization poly methylene poly phenyl poly isocyanate in the present embodiment (referring to accompanying drawing 2, accompanying drawing 3. accompanying drawings 4), it is to be connected with well heater 12 and the output tube by well heater 12 and the airtight flavor still 14 that takes off is welded as a whole by the starting fraction input tube, and tube chamber communicates; Take off flavor still 14 for cylindric, the bottom is the segment shape, and segment end points place processes porose and is welded with output tube 20 and is connected with valve 23 on its outer wall, the input terminus of the output termination water cooler 21 of valve 23, the input terminus of the output termination basin 22 of water cooler 21; Rare gas element input tube 13 stretches into by the mesopore that takes off flavor still 14 loam cakes and takes off in flavor still 14 cavitys, its lower end is welded with three dispersion pipes 15, dispersion pipe 15 tube chambers communicate with rare gas element input tube 13 tube cavities, and uniform in 360 ° of scopes around rare gas element input tube 13; Pipeline 16 is welded on and takes off flavor still 14 loam cakes one side, its the other end inserts the input terminus of condenser 17, outer wall one face down bonding of condenser 17 is connected to pipeline 18 and directly is connected to vacuum extractor, the output terminal of condenser 17 is connected with condensate drum 19 by pipeline, more than constitutes a kind of isolated plant of implementing present embodiment.
Embodiment 2
A kind of production method of polymerization poly methylene poly phenyl poly isocyanate (referring to accompanying drawing 1), its existing production technology is identical with embodiment 1, and purification processes 8 technological processs of its present embodiment, treatment capacity, processing mode are all identical with embodiment 1.Different is: the starting fraction Heating temperature is 150-180 ℃, and vacuum pressure is 0-100mmHg, and the rare gas element of feeding is He, and the He amount is 6Nm 3/ h, the treatment time is 30-100 minute, 45-50 ℃ of discharging chilling temperature.Starting fraction after handling through above-mentioned processing method is through sampling analysis: hydrolyzable chloride content is 0.0023%, and chromatic number 20 platinum cobalts number have no irritating odor, through pressing 1: 1 frothing test with combined polyether glycol, have no irritating odor, condensing liquid quantity is 8.5kg, and hydrolyzable chloride content is 0.1261%.More than can produce the product that polymerization poly methylene poly phenyl poly isocyanate of the present invention has no irritating odor.
Isolated plant in the production method of present embodiment is basic identical with embodiment 1, different is, and (referring to accompanying drawing 5, accompanying drawing 6) rare gas element input tube 13 stretches into by the mesopore that takes off flavor still 14 loam cakes takes off in the flavor still inner chamber, its lower end is welded with 8 dispersion pipes 15, dispersion pipe 15 tube chambers communicate with rare gas element input tube 13 tube cavities, and are double-deck around rare gas element input tube 13 and evenly are dislocatedly distributed in 360 ° of scopes.
Embodiment 3
A kind of production method of polymerization poly methylene poly phenyl poly isocyanate (referring to accompanying drawing 1, accompanying drawing 2), its existing production technology is identical with embodiment 1, other is all inequality, the treating processes of the purification processes 8 of present embodiment is the continous way processing mode, it is that starting fraction is heated to 180-220 ℃ and take off flavor still 14 by pipeline input in well heater 12, its flow is 200kg/h, taking off flavor still 14 is a packing tower, and it is 2Nm that CO gas is input to the bottom of taking off flavor still 14 and the filler by within it to the top CO gas volume of tower by pipeline 13 3/ h, taking off flavor still 14 interior vacuum pressures is between the 200-300mmHg.The residence time is 5-30 minute, and the starting fraction discharging of processing back enters water cooler 21 and carries out the chilling processing, makes it be chilled to 50-60 ℃, enters basin 22 again, is mixed in proportion 10 with first polymerization poly methylene poly phenyl poly isocyanate, after cut; Pipeline 16 enters condensate drum 19 with the light constituent impurity that rare gas element (CO) is carried secretly by tube chamber under the effect of vacuum unit, the treating processes of purification processes 8 is a process continuously.More than can produce the product that polymerization poly methylene poly phenyl poly isocyanate of the present invention has no irritating odor, starting fraction sampling analysis result after treatment: hydrolyzable chloride content is 0.0016%.Chromatic number 10 platinum cobalts number have no irritating odor, and carry out frothing test and have no irritating odor.
Equipment in the production method of present embodiment is relative assembly in the prior art.

Claims (7)

1, a kind of production method of polymerization poly methylene poly phenyl poly isocyanate, it comprises condensation reaction, phosgenation reaction successively, removes phosgene, removes inert solvent, put forward the removal of impurity, flash liberation, secondary separation, hybrid technique process, it is characterized in that this production method is to be provided with the purification processes technological process between secondary separation and hybrid technique process; Described purification processes technological process is that the starting fraction with thick pure diphenylmethanediisocyanate is heated to 120-220 ℃, vacuum pressure is 0-300mmHg in taking off the flavor still, time is under 10-200 minute the condition, disperse to take off flavor by the input rare gas element and handle, be chilled to 40-60 ℃ afterwards and mix with first polymerization poly methylene poly phenyl poly isocyanate again.
2, the production method of polymerization poly methylene poly phenyl poly isocyanate according to claim 1, it is characterized in that described purification processes technological process is that starting fraction with thick pure diphenylmethanediisocyanate is heated to 150-200 ℃, vacuum pressure is 0-100mmHg in taking off the flavor still, time is under 30-100 minute the condition, disperse to take off flavor by the input rare gas element and handle, be chilled to 45-50 ℃ afterwards and mix with first polymerization poly methylene poly phenyl poly isocyanate again.
3, the production method of polymerization poly methylene poly phenyl poly isocyanate according to claim 1 and 2, it is characterized in that described dispersion take off the flavor be treated to the intermittent type processing mode, also can be the continous way processing mode.
4, the production method of polymerization poly methylene poly phenyl poly isocyanate according to claim 1 and 2 is characterized in that described rare gas element is He, N 2, H 2, among the CO any.
5, a kind of isolated plant of method of production polymerization poly methylene poly phenyl poly isocyanate, it is by taking off the flavor still, well heater, condenser, condensate drum, water cooler, the rare gas element basin is connected to one by pipeline and forms, it is characterized in that this isolated plant comprises that taking off the airtight middle part, cavity tank body lower end of flavor still is provided with the hole and is connected with output tube, upper end one side is provided with the input tube that tube chamber communicates and is connected with well heater, opposite side is provided with the output tube that tube chamber communicates and is connected with condenser, upper center is provided with gas inlet pipe and extends takes off flavor still cavity bottom, and its end is provided with at least three and uniform tube chamber communicates in 360 ° of scopes dispersion pipe.
6, isolated plant according to claim 5, it is characterized in that described take off the flavor still up and down two ends be arc structure.
7, isolated plant according to claim 5 is characterized in that described dispersion pipe is the setting of stratiform dislocation type structure.
CN98110586A 1998-11-23 1998-11-23 Process and special equipment for polymerizing polymethanopolyphenyl polyisocyanate Expired - Lifetime CN1099430C (en)

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CN98110586A CN1099430C (en) 1998-11-23 1998-11-23 Process and special equipment for polymerizing polymethanopolyphenyl polyisocyanate

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CN98110586A CN1099430C (en) 1998-11-23 1998-11-23 Process and special equipment for polymerizing polymethanopolyphenyl polyisocyanate

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CN1099430C true CN1099430C (en) 2003-01-22

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5086163A (en) * 1973-12-05 1975-07-11
DD286934A7 (en) * 1988-04-25 1991-02-14 Synthesewerk Schwarzheide Ag,De PROCESS FOR CLEANING ORGANIC ISOCYANATES FROM CHLORINE-CONTAINING COMPOUNDS
US5136087A (en) * 1991-05-15 1992-08-04 Miles Inc. Preparation of polymethylene polyphenyl polyisocyanate
US5312971A (en) * 1992-07-23 1994-05-17 Miles Inc. Color reduction of polymethylene polyphenyl polyisocyanates

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5086163A (en) * 1973-12-05 1975-07-11
DD286934A7 (en) * 1988-04-25 1991-02-14 Synthesewerk Schwarzheide Ag,De PROCESS FOR CLEANING ORGANIC ISOCYANATES FROM CHLORINE-CONTAINING COMPOUNDS
US5136087A (en) * 1991-05-15 1992-08-04 Miles Inc. Preparation of polymethylene polyphenyl polyisocyanate
US5312971A (en) * 1992-07-23 1994-05-17 Miles Inc. Color reduction of polymethylene polyphenyl polyisocyanates

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Free format text: CORRECT: APPLICANT; FROM: YANTAI WANHUA SYNTHETIC LEATHER GROUP CO., LTD TO: YANTAI WANHUA POLYURETHANE CO., LTD.

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Assignee: Ningbo Wanhua Polyurethane Co., Ltd.

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Denomination of invention: Process and special equipment for polymerizing polymethanopolyphenyl polyisocyanate

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