CN103709393B - A kind of method utilizing recovery alcohol and EO to prepare Hydrophilicrto polyether polyvalent alcohol - Google Patents
A kind of method utilizing recovery alcohol and EO to prepare Hydrophilicrto polyether polyvalent alcohol Download PDFInfo
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- CN103709393B CN103709393B CN201310653264.2A CN201310653264A CN103709393B CN 103709393 B CN103709393 B CN 103709393B CN 201310653264 A CN201310653264 A CN 201310653264A CN 103709393 B CN103709393 B CN 103709393B
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Abstract
The invention discloses a kind of method utilizing recovery alcohol and EO to prepare Hydrophilicrto polyether polyvalent alcohol, comprise the following steps: 1) low molecule is reclaimed alcohol, catalyzer etc. and put in reactor, be warmed up to 100 ~ 110 DEG C; 2) logical N
2and slowly drip propylene oxide, keep temperature of reaction at 110 ~ 120 DEG C, stopped reaction after hydroxyl value and target hydroxyl value meet, obtains raw product; 3) raw product is proceeded to refining kettle, add phosphoric acid, finishing agent, generate solid sediment with catalyst action, throw out is filtered, obtain refined products; 4) refined products is heated to 120 DEG C, carry out cooling discharge after vacuum hydro-extraction.The present invention makes full use of the wetting ability of polyether glycol, makes powder puff effectively lock water moisturizing.With the low molecular polylol reclaimed for raw material, production cost is low, can realize the Environmentally-frielow-energy-consumptipolycarboxylic low-energy-consumptipolycarboxylic recycling of useless alcohol simultaneously.
Description
Technical field
The present invention relates to a kind of preparation method of powder puff polyether glycol, especially a kind of method utilizing recovery alcohol and EO to prepare Hydrophilicrto polyether polyvalent alcohol.
Background technology
Polyether glycol is one of important source material of synthesis of polyurethane resin, and it is with the compound of low molecular polylol, polyamine or reactive hydrogen for initiator, forms with olefin oxide ring-opening polymerization under catalyst action.With polyether glycol be that the flexible PU foam density of Material synthesis is low, elastic recovery good, sound-absorbing, the performance such as ventilative, insulation.Flexible PU foam is widely used in mat material, sound-proof material, packing, wrapping material and Fabric composites etc.
Polyether glycol is generally clear viscous liquids, non-volatility, and color is generally colourless, micro-yellow or yellow etc..Than water weight, good hydrophilic property, can mix with water arbitrary proportion.With the powder puff of polyether glycol synthesis of polyurethane, have good flexibility, lock water moisture retention is also fine, also meets environmental protection simultaneously.
At present, the main liquid component of photovoltaic cutting fluid is dibasic alcohol and glycerine, along with the development of photovoltaic cause and petrochemical industry, constantly can produce various polyvalent alcohol waste liquid, therefore, certainly will will consider the subsequent disposal to it.Because the polyvalent alcohol purity reclaimed is not high, cause it to be also subject to a definite limitation in sale and application aspect, but do meticulous purification and greatly can increase tooling cost, not only energy consumption greatly, and processing cost is high.
Summary of the invention
In order to reduce energy consumption, fully represent the polyvalent alcohol added value of recovery, the present invention utilizes and reclaims photovoltaic cutting fluid, reclaims glycol ether and propylene oxide reaction, and prepare the polyether glycol that can meet different customer requirement, concrete steps are as follows:
1) low molecule being reclaimed alcohol, catalyzer etc. puts in reactor, is warmed up to 100 ~ 110 DEG C;
2) N is passed into
2make protection gas, and slowly dropping propylene oxide makes still internal pressure maintain 0.2 ~ 0.3MPa, keep temperature of reaction at 110 ~ 120 DEG C, after reaction for some time, hydroxyl value is surveyed in sampling, and stopped reaction after hydroxyl value and target hydroxyl value meet, obtains raw product;
3) by step 2) obtained raw product proceeds to refining kettle, and add phosphoric acid, finishing agent, the catalyst action allowing itself and step 1) add generates solid sediment, is filtered by throw out, obtains refined products;
4) refined products is heated to 120 DEG C, be evacuated to-0.10Mpa and carry out vacuum hydro-extraction, cooling discharge after each qualified.
Further, described recovery alcohol refers to and reclaims photovoltaic cutting fluid and the alcohol mixture reclaiming low mass molecule alcohol.
Further, described recovery photovoltaic cutting fluid is colourity not higher than the transparent liquid of 50Hazen with recovery low mass molecule alcohol.
Further, it is characterized in that, the mass ratio of described recovery photovoltaic cutting fluid is (10 ~ 60): (10 ~ 60).
Further, the hydroxyl value scope of described recovery photovoltaic cutting fluid is 500 ~ 750mgKOH/g.
Further, content >=90% of described recovery low mass molecule alcohol, and other impurity can be water, or the mixture of water and small molecule polyol.
Further, described small molecule polyol is a kind of dibasic alcohol or multiple dibasic alcohol, and molecular weight is within 200g/mol, and boiling point is less than 300 DEG C.
Further, the content of described small molecule polyol is no more than 5%.
Further, described high temperature and high pressure steam refers to water vapor, and vapor pressure is 1.0 ~ 5.5MPa.
Further, described catalyzer is potassium hydroxide, and accounts for 0.01 ~ 0.03% of all raw material total masses.
Have employed such scheme, obtain a kind of Hydrophilicrto polyether polyvalent alcohol.Powder puff Contents In Polyether Polyol of the present invention reclaims small molecular alcohol and propylene oxide synthesizes, and makes full use of the wetting ability of polyether glycol, makes powder puff effectively lock water moisturizing.Adopt high temperature and high pressure steam heating method, with the low molecular polylol reclaimed for raw material, heating efficiency improves, and production cost is low simultaneously, can realize the Environmentally-frielow-energy-consumptipolycarboxylic low-energy-consumptipolycarboxylic recycling of useless alcohol simultaneously.
The energy consumption of existing type of heating is high, not energy-conservation, and low molecular polylol finished product raw materials cost is high; And the present invention's utilization is the low molecular polylol reclaimed, can accomplish to make the best use of everything, adopt the method for high temperature and high pressure steam heating, environmental protection and energy saving more, production cost is relatively low, and product has more market competition advantage simultaneously.
Embodiment
Below in conjunction with embodiment, the present invention is further detailed explanation.
Embodiment 1:
1) 50Kg is reclaimed in the disposable input reactors such as photovoltaic cutting fluid (hydroxyl value 500mgKOH/g), 12g potassium hydroxide;
2) adopt the method for high temperature and high pressure steam heating, be warming up to 100 DEG C;
3) N is passed into
2make protection gas and keep not interrupting, slowly dripping propylene oxide 74.4kg, control still and be pressed in 0.2 ~ 0.3Mpa, still temperature is at 115 DEG C, and stopped reaction after product hydroxyl value is qualified, obtains raw product;
4) raw product is proceeded to refining kettle, add phosphoric acid, finishing agent produces solid sediment, filter, obtain refined products;
5) refined products is heated to 120 DEG C, be evacuated to-0.10Mpa and carry out vacuum hydro-extraction, stop vacuumizing after each qualified such as moisture, pH value, cooling discharging, namely obtains powder puff polyether glycol (hydroxyl value 37mgKOH/g, moisture 0.03%).
Embodiment 2:
1) 68Kg is reclaimed photovoltaic cutting fluid (hydroxyl value 598mgKOH/g), in the disposable input reactors such as 12g potassium hydroxide;
2) adopt the method for high temperature and high pressure steam heating, be warming up to 100 DEG C;
3) N is passed into
2make protection gas and keep not interrupting, slowly dripping propylene oxide 60.42kg, control still and be pressed in 0.2 ~ 0.3Mpa, still temperature is at 115 DEG C, and stopped reaction after product hydroxyl value is qualified, obtains raw product;
4) raw product is proceeded to refining kettle, add phosphoric acid, finishing agent produces solid sediment, filter, obtain refined products;
5) refined products is heated to 120 DEG C, be evacuated to-0.10Mpa and carry out vacuum hydro-extraction, stop vacuumizing after each qualified such as moisture, pH value, cooling discharging, namely obtains powder puff polyether glycol (hydroxyl value 42mgKOH/g, moisture 0.03%).
Embodiment 3:
1) 80Kg is reclaimed photovoltaic cutting fluid (hydroxyl value 750mgKOH/g), in the disposable input reactors such as 18.7g potassium hydroxide;
2) adopt the method for high temperature and high pressure steam heating, be warming up to 100 DEG C;
3) N is passed into
2make protection gas and keep not interrupting, slowly dripping propylene oxide 107kg, control still and be pressed in 0.2 ~ 0.3Mpa, still temperature is at 115 DEG C, and stopped reaction after product hydroxyl value is qualified, obtains raw product;
4) raw product is proceeded to refining kettle, add phosphoric acid, finishing agent produces solid sediment, filter, obtain refined products;
5) refined products is heated to 120 DEG C, be evacuated to-0.10Mpa and carry out vacuum hydro-extraction, stop vacuumizing after each qualified such as moisture, pH value, cooling discharging, namely obtains powder puff polyether glycol (hydroxyl value 55mgKOH/g, moisture 0.03%).
Embodiment 4:
1) 20Kg is reclaimed in the disposable input reactors such as photovoltaic cutting fluid (hydroxyl value 500mgKOH/g), 4.2g potassium hydroxide;
2) adopt the method for high temperature and high pressure steam heating, be warming up to 100 DEG C;
3) N is passed into
2make protection gas and keep not interrupting, slowly dripping propylene oxide 22.3kg, control still and be pressed in 0.2 ~ 0.3Mpa, still temperature is at 115 DEG C, and stopped reaction after product hydroxyl value is qualified, obtains raw product;
4) raw product is proceeded to refining kettle, add phosphoric acid, finishing agent produces solid sediment, filter, obtain refined products;
5) refined products is heated to 120 DEG C, be evacuated to-0.10Mpa and carry out vacuum hydro-extraction, stop vacuumizing after each qualified such as moisture, pH value, cooling discharging, namely obtains powder puff polyether glycol (hydroxyl value 39mgKOH/g, moisture 0.03%).
Claims (9)
1. utilize recovery alcohol and EO to prepare a method for Hydrophilicrto polyether polyvalent alcohol, it is characterized in that, comprise the following steps:
1) low molecule is reclaimed alcohol, catalyzer puts in reactor, adopt the method for high temperature and high pressure steam heating, be warmed up to 100 ~ 110 DEG C;
2) N is passed into
2make protection gas, and slowly dropping propylene oxide makes still internal pressure maintain 0.2 ~ 0.3MPa, keep temperature of reaction at 110 ~ 120 DEG C, after reaction for some time, hydroxyl value is surveyed in sampling, and stopped reaction after hydroxyl value and target hydroxyl value meet, obtains raw product;
3) by step 2) obtained raw product proceeds to refining kettle, adds phosphoric acid, finishing agent, allows itself and step 1) catalyst action that adds generates solid sediment, throw out is filtered, obtains refined products;
4) refined products is heated to 120 DEG C, be evacuated to-0.10Mpa and carry out vacuum hydro-extraction, cooling discharge after each qualified.
2. a kind of method utilizing recovery alcohol and EO to prepare Hydrophilicrto polyether polyvalent alcohol according to claim 1, is characterized in that, described recovery alcohol refers to and reclaims photovoltaic cutting fluid and the alcohol mixture reclaiming low mass molecule alcohol.
3. a kind of method utilizing recovery alcohol and EO to prepare Hydrophilicrto polyether polyvalent alcohol according to claim 2, it is characterized in that, described recovery photovoltaic cutting fluid is colourity not higher than the transparent liquid of 50Hazen with recovery low mass molecule alcohol.
4. a kind of method utilizing recovery alcohol and EO to prepare Hydrophilicrto polyether polyvalent alcohol according to claim 2, it is characterized in that, the hydroxyl value scope of described recovery photovoltaic cutting fluid is 500 ~ 750mgKOH/g.
5. a kind of method utilizing recovery alcohol and EO to prepare Hydrophilicrto polyether polyvalent alcohol according to claim 2, it is characterized in that, content >=90% of described recovery low mass molecule alcohol, and other impurity is water, or the mixture of water and small molecule polyol.
6. a kind of method utilizing recovery alcohol and EO to prepare Hydrophilicrto polyether polyvalent alcohol according to claim 5, it is characterized in that, described small molecule polyol is a kind of dibasic alcohol or multiple dibasic alcohol, and molecular weight is within 200g/mol, and boiling point is less than 300 DEG C.
7. a kind of method utilizing recovery alcohol and EO to prepare Hydrophilicrto polyether polyvalent alcohol according to claim 5, it is characterized in that, the content of described small molecule polyol is no more than 5%.
8. a kind of method utilizing recovery alcohol and EO to prepare Hydrophilicrto polyether polyvalent alcohol according to claim 1, it is characterized in that, described high temperature and high pressure steam refers to water vapor, and vapor pressure is 1.0 ~ 5.5MPa.
9. a kind of method utilizing recovery alcohol and EO to prepare Hydrophilicrto polyether polyvalent alcohol according to claim 1, it is characterized in that, described catalyzer is potassium hydroxide, and accounts for 0.01 ~ 0.03% of all raw material total masses.
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| CN201310653264.2A CN103709393B (en) | 2013-12-06 | 2013-12-06 | A kind of method utilizing recovery alcohol and EO to prepare Hydrophilicrto polyether polyvalent alcohol |
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| CN103709393B true CN103709393B (en) | 2016-03-02 |
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