CN109705281A - A method of preparing polymer polyatomic alcohol - Google Patents
A method of preparing polymer polyatomic alcohol Download PDFInfo
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- CN109705281A CN109705281A CN201811621177.8A CN201811621177A CN109705281A CN 109705281 A CN109705281 A CN 109705281A CN 201811621177 A CN201811621177 A CN 201811621177A CN 109705281 A CN109705281 A CN 109705281A
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Abstract
The present invention discloses a kind of method for preparing polymer polyatomic alcohol, by styrene in isopropanol solvent, acrylonitrile, macromolcular dispersant, initiator A and polyether polyol mixing obtain raw material flow, under 100-150 DEG C of reaction temperature and under 0.1-0.6Mpa pressure, raw material flow is sent at least three concatenated stirring-type reaction kettles to be reacted, initiator B wherein is added in the second reaction kettle, raw material flow stops 0.5-1.7 hours in each reactor, continuously prepare polymer polyatomic alcohol, make styrene, acrylonitrile reacts with polyether polyol and reacts more complete, improve yield, reduce the energy consumption of post-processing.
Description
Technical field
The present invention relates to a kind of method for preparing polymer polyatomic alcohol, especially multistep continuity method synthesis of high solid content to polymerize
The method of object polyalcohol.
Background technique
Graft polyether (abbreviation POP) is also referred to as polymer polyatomic alcohol, has developed to the third generation so far from last century the seventies.
First generation POP is using acrylonitrile as monomer, solid content 5-20%, and second generation POP replaces part propylene nitrile, solid content with styrene
It is added to polymeric monomer relative to second generation POP, improves grafting rate for 20-30%, third generation POP, stabilizes dispersion, Gu
Content is 40-45%, can satisfy the requirement of high load capacity, high rebound and low compression deformation foamed plastics.
Polymer polyatomic alcohol be based on polyether polyol with the monomer with alkenyl under the initiation of radical initiator
In-situ polymerization occurs, generates the grafted polyether polyol containing solid particle.The polyalcohol contains hydroxyl, has benzene second on side chain
The molecule that the polymer of alkene or acrylonitrile is formed, can carry out polyurethane foam, and foam is made to have better load, increase
Add the hardness of foam
It in patent CN104045773A, is connected using double kettles, is first forming raw material flow lower than mixture under reaction temperature, then to be added dropwise
Mode be added in reactor and reacted, the method stable product quality, product viscosity are lower, while solving reactor knot
Dirt and line clogging problem.
Domestic POP manufacturer also mainly uses two kettle continuous production modes, and first reactor is grafting reactor, and second
Reactor is aging reaction device, is grafted since the initiator of reaction decomposes and initiation reaction at high temperature, in first reactor anti-
Initiator is largely consumed after answering, and remaining styrene and acrylonitrile can not fully reactings.The reaction of two reactor continuity methods
Conversion ratio is generally 93% or so, and reaction conversion ratio is not high, but due to that can produce POP, manufacturer by circulation step
Also pay no attention to the height of reaction conversion ratio.But low reaction rate has the following problems: can make subsequent processes process complications
And material consumption and energy consumption also increase, and the styrene/acrylonitrile residual of final products is also high.
Purification POP product needs high-temperature vacuum distillation, and isopropanol, styrene, the acrylonitrile that will volatilize condense together
Get off, then is handled.Such as in large-scale production, the mixture of condensation removes moisture and impurity etc., is added further according to ratio new
Used in fresh material material (it because styrene, acrylonitrile are volatile injurants, cannot discharge, and be handled as entered waste water system,
Supplies consumption is also increased, therefore condensate liquid must be recycled).In POP continuous production processes, after-treatment system is one
Bigger investment, including distillation, processing and storage equipment, and consume biggish energy consumption.
And if the reaction conversion ratio of styrene, acrylonitrile improves, it can reduce post-processing load, reduce energy consumption and object
Consumption.
Summary of the invention
For high, the low problem of reaction conversion ratio that solves styrene, acrylonitrile residue in the synthesis of previous polymer polyatomic alcohol,
And also to solve the problems, such as that styrene, acrylonitrile high residue bear big, present invention offer caused by subsequent treatment process
It is a kind of by supplement addition initiator in the second reactor, so that the reaction of styrene, acrylonitrile is more completely synthesized Gao Gu
The method of content polymer polyatomic alcohol.
The method of the present invention for preparing polymer polyatomic alcohol, comprising the following steps:
By polyether polyol, styrene, acrylonitrile, macromolcular dispersant, as the chain-transferring agent and initiator A of solvent, low
Mixture is carried out at a temperature of reaction temperature, forms raw material flow；
Raw material flow is sent into concatenated at least three reactor, in 100-150 DEG C of reaction temperature and 0.1-0.6Mpa pressure
Lower reaction, wherein be added has an initiator B in the second reactor, raw material flow stops 0.5-1.7 hours in each reactor, most
Polymer polyatomic alcohol is obtained from the discharging of third reactor afterwards.
Preferably, the polyether polyol contains propylene oxide and ethylene oxide chain, molecular weight 2000-6000, epoxy
Ethane content is 7-15%, hydroxy functionality 3.
Preferably, the styrene: the mass ratio of acrylonitrile is 1:9-6:4, and the mixture of styrene and acrylonitrile accounts for poly-
The 40-110% of ethoxylated polyhydric alcohol quality.
Preferably, the macromolcular dispersant be selected from maleic acid, maleic anhydride, fumaric acid, fumaric acid anhydride it is any
Unsaturated acids and hydroxyl macromolecule polyether reactant, then the compound synthesized with reacting ethylene oxide, macromolecular dispersion
Agent accounts for the 6-10% of polyether polyol quality.
Preferably, the chain-transferring agent as solvent is selected from toluene, ethylbenzene, hexane, butanol, isobutanol, isopropanol, second
Acetoacetic ester, mercaptan it is one or more, account for 9% or more of polyether polyol quality as the chain-transferring agent of solvent.
Preferably, the initiator A, initiator B are selected from benzoyl peroxide, dual-tert-butyl cyclohexane peroxide, double
Tert-butyl hydroperoxide pentamethylene, azodiisobutyronitrile it is any；Initiator A accounts for the 0.1-5% of polyether polyol quality, preferably
0.6-0.1%, initiator B account for the 0.05-0.5% of polyether polyol quality, preferably 0.06-0.1%.
Preferably, the initiator A is azodiisobutyronitrile, and initiator B is dual-tert-butyl peroxidating pentamethylene.
Preferably, raw material flow residence time in each reactor is 1 hour.
The utility model has the advantages that the present invention passes through three concatenated reactors of setting, and initiator is added in the second reactor, together
When stop raw material flow 0.5-1.7 hours in each reactor so that styrene, the residual quantity of acrylonitrile are big in final product
Width is reduced, and improves reaction conversion ratio, conversion ratio 3-4% can be improved by secondary initiation reaction, final conversion ratio is made to reach 97%
Left and right reduces energy consumption and material consumption to substantially mitigate post-processing load.
Detailed description of the invention
Fig. 1 is the electromicroscopic photograph (6000 times) of the POP in the three kettles synthesis of embodiment 2 after supplement initiator.
Fig. 2 is the electromicroscopic photograph (6000 times) for not supplementing the POP of initiator during two kettles of comparative example 2 synthesize.
Specific embodiment
Technical solution of the present invention is described in detail below by embodiment, but protection scope of the present invention is not limited to
In the embodiment.
The of the invention method for preparing polymer polyatomic alcohol the following steps are included:
By polyether polyol, styrene, acrylonitrile, macromolcular dispersant, as the chain-transferring agent and initiator A of solvent, low
Mixture is carried out at a temperature of reaction temperature, forms raw material flow；
Raw material flow is sent into concatenated at least three reactor, in 100-150 DEG C of reaction temperature and 0.1-0.6Mpa pressure
Lower reaction, wherein be added has an initiator B in the second reactor, raw material flow stops 0.5-1.7 hours in each reactor, most
Polymer polyatomic alcohol is obtained from the discharging of third reactor afterwards.
Above-mentioned polyether polyol is the addition product of epoxide and polyol, suitable epoxide example
It is such as selected from propylene oxide, ethylene oxide and its mixture, suitable polyol is for example selected from glycerine, trihydroxy methyl
Propane, pentaerythrite, propylene glycol etc..In a preferred embodiment, polyether polyol is using glycerine as initiator and epoxy third
Alkane, ethylene oxide mix alkane reaction and prepare, and propylene oxide and the ethylene oxide chain of polyether polyol can be hybrid mode or embedding
The segment of segmented mode；The polyether polyol molecular weight of preparation is 2000-6000, and wherein ethylene oxide content is 7-15%, hydroxyl official
Energy degree is 3.
The mass ratio of above-mentioned styrene and acrylonitrile is 1:9-6:4, preferably 7:3-6:4, styrene and acrylonitrile it is mixed
Close 40-110%, preferably 60-90% that object total amount accounts for polyether polyol quality.
Above-mentioned macromolcular dispersant is that the compound of acid containing unsaturated double-bond and the macromolecule polyethers of hydroxyl exist
The compound synthesized again with reacting ethylene oxide after being reacted at a temperature of 120 DEG C or so.Acid containing unsaturated double-bond is selected from Malaysia
Any, preferred maleic anhydride of acid or maleic anhydride, fumaric acid or fumaric acid anhydride.The macromolecule polyethers of hydroxyl is molecule
The high rebound polyethers that amount is 4800-5000 or so, such as the manufacture of the Nanjing polyethers NJ-330N(Ningwu chemical plant).Preferably at one
It is in scheme, maleic anhydride (Dow manufacture) is anti-after 120 DEG C or so are reacted, then with ethylene oxide with polyethers NJ-330N
It answers and prepares macromolcular dispersant, wherein the molar ratio of NJ-330N and maleic anhydride and ethylene oxide is 1:1:1, and gained divides greatly
The acid value of sub- dispersing agent is less than 0.5mgKOH/g.Macromolcular dispersant accounts for the 6-10% of polyether polyol quality, preferably 6-8%.
Above-mentioned chain-transferring agent can double as solvent, be selected from toluene, ethylbenzene, hexane, butanol, isobutanol, isopropanol, acetic acid second
Any one or more, the preferred isopropanol of ester, mercaptan.When as chain-transferring agent, chain-transferring agent accounts for polyether polyol quality
9% or more；When as solvent, quantity of solvent is not particularly limited.But if the solvent being added is excessive, then it is also needed to steam in product
It distillates and, more energy consumptions can be consumed, therefore the amount that solvent is added is preferably the 9-10% of polyether polyol quality, in this way, both may be used
Meet the requirement that can meet again as chain-transferring agent as solvent.
Above-mentioned initiator can be any for causing the radical initiator of polymerization.Preferably radical initiator includes
But it is not limited to: peroxide type organic (such as benzoyl peroxide, dual-tert-butyl cyclohexane peroxide, dual-tert-butyl peroxide
Change pentamethylene) and azo-compound (such as azodiisobutyronitrile).It is short from thermal decomposition half life and reaction monomers can be made as early as possible
To polymer conversion, and from the point of view of the aspect that is easily dissolved in styrene and acrylonitrile, draw what raw material mix stages used
Sending out agent A is preferably azodiisobutyronitrile (solid white powder), and initiator A accounts for the 0.1-5% of polyether polyol quality.The reason is that
During reacting under the above-described reaction conditions, initiator gradually resolves into free radical, initiated polymerization, and is consumed, when
When the concentration of initiator is more than 5%, apparent autohemagglutination or mixed poly-, polyether polyols can occur for styrene and acrylonitrile in reaction raw materials
The rate of alcohol and styrene, acrylonitrile polymerization is lower than autohemagglutination rate, and obtained POP is mainly ex situ polymerization, makes runaway reaction,
Generate cohesion, the particle in POP is easy sedimentation, store it is unstable, poor product quality and can not normal use；It is dense when initiator
When degree is lower than 0.1%, polyether polyol and styrene, acrylonitrile reactor are incomplete, cause unreacted styrene, acrylonitrile residual
It stays and increases.Initiator A preferably accounts for the 0.6-1% of polyether polyol quality.
From improve second reactor in styrene, acrylonitrile reactor conversion ratio in terms of, in the second reactor
The initiator B used is preferably that dual-tert-butyl peroxidating pentamethylene (dissolves dual-tert-butyl peroxidating ring by isopropanol when using
Solution made of pentane).Initiator B accounts for the 0.05-0.5% of polyether polyol quality, preferably 0.06-0.1%.
The present invention uses the tandem reaction kettle of at least three same volumes, and the temperature for controlling three reaction kettles is 100-150
DEG C, preferably 125-135 DEG C, pressure 0.2-0.6Mpa, preferably 0.35-0.45Mpa, by raw material flow be pumped into first instead
It answers kettle to be reacted, after raw material is full of the first reaction kettle, into the second reaction kettle, micro draw is added in the second reaction kettle
Agent is sent out, the reaction was continued, and third reaction kettle is entered after the second reaction kettle is full of, and the reaction was continued (or being aging reaction), passes through
Discharging obtains the crude product of POP after aging reaction.It is sent into the flow velocity of reaction kettle, about raw material flow can stop in each reaction kettle
Subject to 0.5-1.7 hours.
When residence time is more than 1.7 small to raw material flow in a kettle, not only reaction conversion ratio will not continue to increase, and
And also will affect the viscosity of final product, influence using；If residence time is less than 0.5 hour raw material flow in a kettle,
Then reaction conversion ratio declines, and residual reactants are higher.The residence time of raw material flow in a kettle is preferably 1 hour, at this time instead
It answers sufficiently, high conversion rate, obtained product viscosity is moderate.
Conversion ratio 3-4% can be improved by secondary initiation reaction, and so on, it is further added by initiation reaction number, graft reaction
It can be more complete.But considers the investment of energy consumption and equipment, carry out secondary or initiation grafting reaction three times, residual reactants can be made to reach
To desirable balance point.
Experimental rig and technique:
Experimental rig, which is a head tank, passes through the micro pump of adjustable flow and three concatenated 0.5L reacting with agitating device
Kettle is connected, and three reaction kettle band heating devices simultaneously can auto-adjustment control temperature of charge and pressure.
Raw material flow from the low entrance of kettle and enters back into next reactor bottom from the top discharge of kettle, in the second reactor bottom
The second reaction kettle can be added by the micro pump of adjustable flow in liquid initiator by feed inlet, from top after secondary initiation grafting reaction
Portion's discharging enters back into third reaction kettle and carries out aging reaction, and gas-liquid separator, gas-liquid are entered after third reaction kettle top discharge
System is set to keep discharging after steady pressure, gas-liquid separator are cooling with nitrogen sealing gland on separator, each kettle discharging has sampling
Mouthful.React sample can continuous feed, initiator B can also be continuously added to be reacted in raw material flow.
In following examples, the commercially available product used is as follows:
Styrene (purity is greater than 99.5%, the manufacture of Zhenghai petrochemical industry)；Acrylonitrile (purity is greater than 99.5%, Anqing Petrochemical Company manufacture)；It is different
Propyl alcohol (Dow manufacture)；Azodiisobutyronitrile (manufacture of Tangshan Chen Hong Industrial Co., Ltd.)；Dual-tert-butyl peroxidating ring penta
Alkane (manufacture of Lanzhou auxiliary reagent factory).
Embodiment 1:
It at normal temperatures and pressures, will be as 100 mass parts of polyether polyol of reaction raw materials, 57 mass of styrene in mixed kettle
Part, 28 mass parts of acrylonitrile, 0.66 mass parts of 8 mass parts of macromolcular dispersant, 10 mass parts of isopropanol and azodiisobutyronitrile
It is mixed, and is completely dissolved solid azodiisobutyronitrile, obtain uniform raw material flow, and be added in raw material storage tank.
In order to guarantee that there is uniform temperature and pressure in reaction kettle, appropriate isopropanol is injected with micro pump connect in advance
The first, second, third reaction kettle in, start to stir, open third kettle discharging enter gas-liquid separator valve.Control reaction
Kettle temperature degree is 125-135 DEG C, pressure 0.35-0.45Mpa switches raw material storage tank and be sent into raw material flow instead after the system stabilizes
Kettle is answered to start to react, the flow velocity of raw material flow is 5ml/min(small corresponding to the residence time of raw material flow in a kettle about 1.7
When)；Meanwhile the dual-tert-butyl peroxidating pentamethylene of 0.1 mass parts is made of isopropanol solvent 1% solution, infused with micro pump
Enter the second reactor bottom pipeline and raw material flow is mixed into the second reaction kettle and carries out secondary initiation reaction.After reaction three hours
It is sampled in sample tap, detects remaining styrene, acrylonitrile content in reactant, then started collection separator and go out material
POP, the feed liquid of collection will volatilize object removing, carry out viscosity, mobility, solid content and Electronic Speculum particle detections by vacuum distillation,
It is shown in table 1 to will test tables of data.
Embodiment 2:
Embodiment 1 is repeated, the flow control for entering reaction kettle is corresponded into raw material flow stopping in a kettle in 8.5ml/min(
Stay the time about 1 hour), it is sampled after three hours, and collect POP crude product, performance detection is carried out after vacuum distillation, will test tables of data
It is shown in table 1.
Embodiment 3:
Embodiment 1 is repeated, the flow control for entering reaction kettle is corresponded into the stop of raw material flow in a kettle in 17ml/min(
About 0.5 hour time), it is sampled after three hours, and collect POP crude product, performance detection is carried out after vacuum distillation, will test tables of data
It is shown in table 1.
Comparative example 1:
It at normal temperatures and pressures, will be as 100 mass parts of polyether polyol of reaction raw materials, 57 mass of styrene in mixed kettle
Part, 28 mass parts of acrylonitrile, 0.66 mass parts of 8 mass parts of macromolcular dispersant, 10 mass parts of isopropanol and azodiisobutyronitrile
It is mixed, and is completely dissolved solid azodiisobutyronitrile, obtain uniform raw material flow, be added in raw material storage tank.
In order to guarantee that there is uniform temperature and pressure in reaction kettle, appropriate isopropanol is injected with micro pump connect in advance
The first, second reaction kettle in, start to stir and open the valve of two kettles discharging air inlet liquid/gas separator, make it directly into separation
Device.Control temperature of reaction kettle be 125-135 DEG C, pressure 0.35-0.45Mpa, after the system stabilizes, switching raw material storage tank will be former
Stream is sent into reaction kettle and starts to react, and the flow velocity of raw material flow is that 5ml/min(corresponds to the residence time of raw material flow in a kettle
About 1.7 hours).Reaction is sampled after three hours in sample tap, detects remaining styrene, acrylonitrile content in reactant,
Then start collection separator and go out material POP, the feed liquid of collection will volatilize object removing, carried out viscosity, flowed by vacuum distillation
Property, solid content and Electronic Speculum particle detections, it is shown in table 1 to will test tables of data.
Comparative example 2:
Comparative example 1 is repeated, the flow control for entering reaction kettle is corresponded into raw material flow stopping in a kettle in 8.5ml/min(
Stay the time about 1 hour), it is sampled after three hours, and collect POP crude product, performance detection is carried out after vacuum distillation, will test tables of data
It is shown in table 1.
Comparative example 3:
Comparative example 1 is repeated, the flow control for entering reaction kettle is corresponded into the stop of raw material flow in a kettle in 17ml/min(
About 0.5 hour time), it is sampled after three hours, and collect POP crude product, performance detection is carried out after vacuum distillation, will test tables of data
It is shown in table 1.
Performance detection
Hydroxyl value: it is detected using national standard GB/T 7383-2007；
Styrene, acrylonitrile content: the headspace autosampler (model: 7697A) and gas phase color of Agilent company of the U.S. are used
Spectrometer (model: 7890B), detects its content using general detection method；
Viscosity: it is detected using DJ-N79 rotational viscometer (upper seamark Zhuo scientific instrument Co., Ltd)；
Mobility: the screen filtration by 100g POP sample isopropanol to 50% again through 700 mesh, the time being sieved；
Solid content: weigh 1g sample be added centrifuge tube in and be added 6ml ethyl alcohol be uniformly mixed, in centrifuge (model: TG-1650-
WS, Shanghai Lu Xiang Instrument Ltd.) in centrifugation 20min are turned with 9000-10000, then take out test tube, take out supernatant, stay
Lower white precipitate, then plus 6ml ethyl alcohol, continue above step, washed put remaining white precipitate in an oven in 80-90 three times
DEG C baking about 48 hours, white powder is obtained, the percentage of the quality for weighing powder and sample total amount is solid content.
Above-mentioned testing result is shown in table 1.
Table 1
According to table 1, illustrate during POP same reaction, the average conversion styrene by an initiation reaction is 89-
94% or so, acrylonitrile 90.1-94% is 92.5-96.7% or so, acrylonitrile by secondary initiation average conversion styrene
Reaction efficiency 3-4% therefore can be improved carrying out initiation grafting reaction twice for 93.7-97.5%.
Above data illustrates that the conversion ratio of residence time identical embodiment is above comparative example, while also turning out that reaction stops
It stays the time to be affected conversion ratio, but when the residence time is more than 1.7 hours, will affect the viscosity of final product, influence
It uses, and when the residence time was less than 0.5 hour, conversion ratio is low, and residual reactants are higher.Residence time was on 1 hour left side
The right side, reacts more abundant, high conversion rate, and obtained product viscosity is moderate.
It selects the product of embodiment 2 and comparative example 2 to carry out Electronic Speculum observation, and carries out the comparison of electromicroscopic photograph.
Fig. 1 is the electromicroscopic photograph (6000 times) of product after supplement initiator in the three kettles synthesis of embodiment 2, and Fig. 2 is to compare
The electromicroscopic photograph (6000 times) of the product of initiator is not supplemented in the two kettles synthesis of example 2.It can be seen that embodiment from Fig. 1 and Fig. 2
The electromicroscopic photograph particle surface of 2 secondary grafting reactor product is smooth, and the coacervation of particle is unobvious, and stability is preferable；And
Do not add the product particle surface of supplement initiator smooth in comparative example 2, viscosity also complies with requirement, but has meeting between a small amount of particle
Coacervation is generated, this has certain influence to the stability of product, and long-term storage can coagulative precipitation.
As described above, must not be explained although the present invention has been indicated and described referring to specific preferred embodiment
For the limitation to invention itself.It without prejudice to the spirit and scope of the invention as defined in the appended claims, can be right
Various changes can be made in the form and details for it.
Claims (8)
1. a kind of method for preparing polymer polyatomic alcohol, which comprises the following steps:
By polyether polyol, styrene, acrylonitrile, macromolcular dispersant, as the chain-transferring agent and initiator A of solvent, low
Mixture is carried out at a temperature of reaction temperature, forms raw material flow；
Raw material flow is sent into concatenated at least three reactor, in 100-150 DEG C of reaction temperature and 0.1-0.6Mpa pressure
Lower reaction, wherein be added has an initiator B in the second reactor, raw material flow stops 0.5-1.7 hours in each reactor, most
Polymer polyatomic alcohol is obtained from the discharging of third reactor afterwards.
2. the method according to claim 1 for preparing polymer polyatomic alcohol, which is characterized in that the polyether polyol contains
Propylene oxide and ethylene oxide chain, molecular weight 2000-6000, ethylene oxide content 7-15%, hydroxy functionality 3.
3. the method according to claim 1 for preparing polymer polyatomic alcohol, which is characterized in that the styrene: acrylonitrile
Mass ratio be 1:9-6:4, the mixture of styrene and acrylonitrile accounts for the 40-110% of polyether polyol quality.
4. the method according to claim 1 for preparing polymer polyatomic alcohol, which is characterized in that the macromolcular dispersant is
Selected from maleic acid, maleic anhydride, fumaric acid, fumaric acid anhydride any unsaturated acids and hydroxyl macromolecule polyethers it is anti-
It answers, then the compound synthesized with reacting ethylene oxide, macromolcular dispersant accounts for the 6-10% of polyether polyol quality.
5. the method according to claim 1 for preparing polymer polyatomic alcohol, which is characterized in that the chain as solvent turns
Move agent be selected from toluene, ethylbenzene, hexane, butanol, isobutanol, isopropanol, ethyl acetate, mercaptan it is one or more, double as solvent
Chain-transferring agent account for 9% or more of polyether polyol quality.
6. the method according to claim 1 for preparing polymer polyatomic alcohol, which is characterized in that the initiator A, initiator
B is selected from benzoyl peroxide, dual-tert-butyl cyclohexane peroxide, dual-tert-butyl peroxidating pentamethylene, azodiisobutyronitrile
It is any；Initiator A accounts for the 0.1-5% of polyether polyol quality, and initiator B accounts for the 0.05-0.5% of polyether polyol quality.
7. the method according to claim 6 for preparing polymer polyatomic alcohol, which is characterized in that the initiator A is azo
Bis-isobutyronitrile, initiator B are dual-tert-butyl peroxidating pentamethylene.
8. the method according to claim 1 for preparing polymer polyatomic alcohol, which is characterized in that raw material flow is in each reactor
The middle residence time is 1 hour.
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| CN114505306A (en) * | 2021-12-30 | 2022-05-17 | 云锡文山锌铟冶炼有限公司 | Method for cleaning scale in sulfur dioxide reduction leaching kettle |
| CN115073753A (en) * | 2022-04-08 | 2022-09-20 | 中国石油化工股份有限公司 | Preparation method of polymer polyol |
| CN115141366A (en) * | 2021-03-30 | 2022-10-04 | 中国石油化工股份有限公司 | Method for improving safety of maleic anhydride macromonomer in synthesis process and application |
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