CN112430318A - Safe and efficient water reducing agent polyether production process - Google Patents
Safe and efficient water reducing agent polyether production process Download PDFInfo
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- CN112430318A CN112430318A CN202011134305.3A CN202011134305A CN112430318A CN 112430318 A CN112430318 A CN 112430318A CN 202011134305 A CN202011134305 A CN 202011134305A CN 112430318 A CN112430318 A CN 112430318A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2642—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds characterised by the catalyst used
- C08G65/2645—Metals or compounds thereof, e.g. salts
- C08G65/2648—Alkali metals or compounds thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2603—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen
- C08G65/2606—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups
- C08G65/2609—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups containing aliphatic hydroxyl groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2696—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds characterised by the process or apparatus used
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/30—Post-polymerisation treatment, e.g. recovery, purification, drying
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- Polyethers (AREA)
Abstract
The invention discloses a safe and efficient water reducing agent polyether production process, which comprises the following steps: firstly discharging unqualified liquid potassium hydroxide in a metering tank to a ton barrel for standby, paying attention to the fact that the residual part of a pipeline needs to be removed, adding water to clean twice after material returning, blowing to be qualified, feeding again, reporting and checking again after feeding to ensure that the indexes of raw materials are qualified, (secondly) correcting a catalyst feeding flowmeter FQC-1201-1 to ensure accurate metering, (thirdly) producing 1 batch of HPEG2400 finished products according to the current process formula (sodium methoxide), sampling to be application performance and reserving samples after neutralization and absorption are qualified, reducing manual feeding operation after changing the sodium methoxide into the liquid potassium hydroxide by adopting the production process designed by the invention, avoiding material contact, improving operation safety, ensuring that the reaction can be promoted because the liquid potassium hydroxide and the sodium methoxide belong to strong base substances, and the liquid potassium hydroxide is cheaper than the solid sodium methoxide, the production cost can be reduced.
Description
Technical Field
The invention relates to the technical field of water reducing agents, in particular to a safe and efficient production process of water reducing agent polyether.
Background
In the existing process for producing the water reducing agent polyether, solid sodium methoxide is used as a catalyst, the sodium methoxide is easily combustible when wet, in southern areas, the air humidity is high, the rainy season is more, certain operation risk exists, dust of the sodium methoxide has strong irritation and corrosivity to respiratory tracts, after the sodium methoxide is inhaled, lethargy, central inhibition and anesthesia can be caused, strong irritation and corrosivity to eyes can cause blindness, skin can be contacted and burned, the use risk of the sodium methoxide is high, and the production cost is also high.
Disclosure of Invention
The invention aims to provide a safe and efficient water reducer polyether production process, which has the advantage of high safety and solves the problems that solid sodium methoxide is used as a catalyst in the traditional process for producing water reducer polyether, so that the risk is high and the production cost is high.
In order to achieve the purpose, the invention provides the following technical scheme: a safe and efficient water reducer polyether production process comprises the following steps:
firstly, discharging the original unqualified liquid potassium hydroxide of the metering tank to a ton barrel for standby, paying attention to the fact that the residual part of a pipeline needs to be removed, adding water for cleaning twice after material returning, purging for qualification, feeding again, and reporting to examine again after feeding to ensure that the indexes of raw materials are qualified.
And (II) correcting the catalyst feeding flow meter FQC-1201-1 to ensure accurate metering.
Thirdly, 1 batch of HPEG2400 finished products are produced according to the current process formula (sodium methoxide), and samples are taken as application properties and reserved as reference samples after neutralization and absorption are qualified; then adding a polymerization inhibitor, stirring and circulating for 0.5 hour, sampling again, reserving a sample, reserving a ton of stack, reserving the sample and tracking.
(IV) according to the trial process formula, using liquid potassium hydroxide as a catalyst to produce 2 batches of HPEG2400 finished products, and the main process flow is as follows:
pretreatment: degassing and displacing, feeding an initiator, feeding a catalyst, dehydrating in vacuum, and transferring;
a reactor: adjusting initial reaction conditions, feeding EO in the reaction, curing (for the first production, curing and the like), and transferring materials;
and (3) post-treatment: stripping, cooling, adding acetic acid, neutralizing, absorbing (keeping a sample for stability test after qualified), adding a polymerization inhibitor (sampling and keeping a sample for application performance after stirring for 0.5 h), cooling, and discharging to a tank in the same day.
Sampling the first batch after neutralization and absorption are qualified, taking application performance and keeping samples for testing the stability without adding the polymerization inhibitor, and taking the sampling after adding the polymerization inhibitor, taking application performance and keeping samples, wherein the specific amount of the samples is determined by TS; and then turning to a day tank V12001D to-be-applied performance analysis result, after the to-be-applied performance is tested, evaluating whether the to-be-applied performance meets the product standard of sodium methoxide production by TS, slicing, taking 1 pile in the middle as a pile sample, performing stability tracking, and tracking the use feedback condition of customers by the rest 25 tons.
And (VI) sampling in the second batch and after the absorption is qualified to obtain application performance and reserve the sample, adding a polymerization inhibitor, stirring and circulating for 0.5 hour, then sampling again to reserve the sample, specifically reserving a small amount of sample determined by TS, then turning to a day tank V12001C to wait for an application performance analysis result, after the application performance is tested, evaluating whether the sample meets the product standard of sodium methoxide production by TS, turning to a slice loading tank, continuing to slice the first batch, taking a middle 1 stack as a stack for reserving the sample, performing stability tracking, directionally selling the rest 25 tons or so, and tracking the use feedback condition of a client.
Preferably, the process formula in the fourth step is tried, and the first solution is added into the formula per batch per 5765kg, the KOH (48%)/33.3 kg, the EO/20180kg and the acetic acid per 29 kg.
Preferably, the control of the pretreatment water in the fourth step can be properly relaxed to be less than or equal to 0.08 percent, the water content of the two batches of pretreatment produced in the test is 0.08 percent, the dehydration temperature of the first batch (076A) is 101-.
Preferably, the pretreatment dehydration control in the fourth step requires that roots is started to carry out vacuum strengthening on one hand, and the temperature can be properly increased upwards to shorten the dehydration time on the other hand, but the dehydration temperature is preferably not more than 126.2 ℃ (the current head aging temperature is 124.2-126.2 ℃).
Preferably, in the fourth step, in the later stage of the reaction in the reactor, the feeding amount is about 14 tons, the temperature of the reactor tends to rise, and the prior intervention is required as in the normal batch.
Compared with the prior art, the invention has the following beneficial effects:
1. by adopting the production process designed by the invention, after the catalyst is changed from sodium methoxide to liquid potassium hydroxide, the manual feeding operation is reduced, the contact of materials is avoided, the operation safety is improved, the liquid potassium hydroxide and the sodium methoxide belong to strong base substances and can promote the reaction, the liquid potassium hydroxide is cheaper than solid sodium methoxide in market price, and the production cost can be reduced.
2. At present, the market price of sodium methoxide is 17000 yuan/ton, the addition amount of each batch is 16kg, and the cost is 272 yuan; the price of the liquid potassium hydroxide is 4400 yuan/ton, the addition amount of each batch is 33.3kg, and the cost is about 146.52 yuan, so that the cost of each batch of raw materials can be saved by 125.48 yuan when the liquid potassium hydroxide is used for production.
Drawings
FIG. 1 is a monitoring diagram of the dehydration process of 076A according to the present invention;
FIG. 2 is a monitoring diagram of the dehydration process of 079A according to the present invention;
FIG. 3 is a diagram of the monitoring of the 076A reaction process according to the present invention;
FIG. 4 is a diagram of the monitoring of the 079A reaction process according to the present invention;
FIG. 5 is a table of HPEG2400 product indicator conditions tested in accordance with the present invention;
FIG. 6 is a table showing the application properties of the product of the present invention (neat paste fluidity test, water reducing agent mixing amount 0.60 g).
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a technical scheme that:
a safe and efficient water reducer polyether production process comprises the following steps:
firstly, discharging the original unqualified liquid potassium hydroxide of the metering tank to a ton barrel for standby, paying attention to the fact that the residual part of a pipeline needs to be removed, adding water for cleaning twice after material returning, purging for qualification, feeding again, and reporting to examine again after feeding to ensure that the indexes of raw materials are qualified.
And (II) correcting the catalyst feeding flow meter FQC-1201-1 to ensure accurate metering.
Thirdly, 1 batch of HPEG2400 finished products are produced according to the current process formula (sodium methoxide), and samples are taken as application properties and reserved as reference samples after neutralization and absorption are qualified; then adding a polymerization inhibitor, stirring and circulating for 0.5 hour, sampling again, reserving a sample, reserving a ton of stack, reserving the sample and tracking.
(IV) according to the trial process formula, using liquid potassium hydroxide as a catalyst to produce 2 batches of HPEG2400 finished products, and the main process flow is as follows:
pretreatment: degassing and displacing, feeding an initiator, feeding a catalyst, dehydrating in vacuum, and transferring;
a reactor: adjusting initial reaction conditions, feeding EO in the reaction, curing (for the first production, curing and the like), and transferring materials;
and (3) post-treatment: stripping, cooling, adding acetic acid, neutralizing, absorbing (keeping a sample for stability test after qualified), adding a polymerization inhibitor (sampling and keeping a sample for application performance after stirring for 0.5 h), cooling, and discharging to a tank in the same day.
Sampling the first batch after neutralization and absorption are qualified, taking application performance and keeping samples for testing the stability without adding the polymerization inhibitor, and taking the sampling after adding the polymerization inhibitor, taking application performance and keeping samples, wherein the specific amount of the samples is determined by TS; and then turning to a day tank V12001D to-be-applied performance analysis result, after the to-be-applied performance is tested, evaluating whether the to-be-applied performance meets the product standard of sodium methoxide production by TS, slicing, taking 1 pile in the middle as a pile sample, performing stability tracking, and tracking the use feedback condition of customers by the rest 25 tons.
(VI) sampling in the second batch after the neutralization and absorption are qualified, making application performance and reserving samples, adding a polymerization inhibitor, stirring and circulating for 0.5 hour, then sampling again for reserving samples, specifically reserving a small amount of samples according to TS, then turning to a day tank V12001C to wait for application performance analysis results, after the application performance is tested, evaluating whether the samples meet the product standard of sodium methoxide production according to TS, then turning to a slice loading tank, continuing slicing in the first batch, taking 1 pile in the middle as a pile of reserved samples, performing stability tracking, directionally selling the rest 25 tons, and tracking the feedback condition of the customers; the process formula is tried in the fourth step, wherein heads/5765 kg, KOH (48%)/33.3 kg, EO/20180kg and acetic acid/29 kg are added into each batch, the water content control of the pretreatment in the fourth step can be properly widened to be less than or equal to 0.08%, the water content of the pretreatment in the two batches in the test production is 0.08%, the dehydration temperature of the first batch (076A) is 101-, as with the normal batch, which requires prior intervention, the first batch (076A) has a reaction set point temperature of 124.2-126.2 ℃ and a maximum feed flow rate of 700+4300 kg/h. The PID of the PIC1334 at the early stage of the whole reaction process is set to be 90, 700 and 1.0, the whole temperature fluctuation is larger and becomes a dispersion trend, the PID is adjusted to be 120, 670 and 135, the whole temperature fluctuation is obviously reduced and becomes a convergence trend, no obvious difference exists between the adjusted PID and a normal production batch, the reaction set temperature of the second batch (079A) is 124.2-126.2 ℃, and the maximum feeding flow rate is 700+4300 kg/h. The PID settings of the PIC1334 were produced directly at 120, 670, 135, without fluctuations like the first lot, and without significant differences from the normal production lots.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. A safe and efficient production process of water reducer polyether is characterized by comprising the following steps: the method comprises the following steps:
firstly, discharging unqualified liquid potassium hydroxide originally in a metering tank to a ton barrel for standby, paying attention to the fact that the residual part of a pipeline needs to be removed, adding water for cleaning twice after material returning, blowing and sweeping for qualification, then feeding again, and reporting for inspection after feeding again to ensure that the indexes of raw materials are qualified;
secondly, correcting a catalyst feeding flow meter FQC-1201-1 to ensure accurate metering;
thirdly, 1 batch of HPEG2400 finished products are produced according to the current process formula (sodium methoxide), and samples are taken as application properties and reserved as reference samples after neutralization and absorption are qualified; then adding a polymerization inhibitor, stirring and circulating for 0.5 hour, sampling again, reserving a sample, reserving a ton of stack, reserving the sample and tracking;
(IV) according to the trial process formula, using liquid potassium hydroxide as a catalyst to produce 2 batches of HPEG2400 finished products, and the main process flow is as follows:
pretreatment: degassing and displacing, feeding an initiator, feeding a catalyst, dehydrating in vacuum, and transferring;
a reactor: adjusting initial reaction conditions, feeding EO in the reaction, curing (for the first production, curing and the like), and transferring materials;
and (3) post-treatment: stripping, cooling, adding acetic acid, neutralizing and absorbing (keeping a sample for stability test after the sample is qualified), adding a polymerization inhibitor (sampling and keeping a sample for application performance after stirring for 0.5 h), cooling, and discharging to a day tank;
sampling the first batch after neutralization and absorption are qualified, taking application performance and keeping samples for testing the stability without adding the polymerization inhibitor, and taking the sampling after adding the polymerization inhibitor, taking application performance and keeping samples, wherein the specific amount of the samples is determined by TS; then, transferring a to-be-applied performance analysis result of the day tank V12001D, after the to-be-applied performance is tested, evaluating whether the to-be-applied performance analysis result meets the product standard of sodium methoxide production by TS, slicing, taking the stack 1 in the middle as a stack sample, performing stability tracking, and tracking the use feedback condition of customers by the rest 25 tons;
and (VI) sampling in the second batch and after the absorption is qualified to obtain application performance and reserve the sample, adding a polymerization inhibitor, stirring and circulating for 0.5 hour, then sampling again to reserve the sample, specifically reserving a small amount of sample determined by TS, then turning to a day tank V12001C to wait for an application performance analysis result, after the application performance is tested, evaluating whether the sample meets the product standard of sodium methoxide production by TS, turning to a slice loading tank, continuing to slice the first batch, taking a middle 1 stack as a stack for reserving the sample, performing stability tracking, directionally selling the rest 25 tons or so, and tracking the use feedback condition of a client.
2. The safe and efficient water reducer polyether production process according to claim 1, characterized in that: in the process formula tested in the fourth step, heads/5765 kg, KOH (48%)/33.3 kg, EO/20180kg and acetic acid/29 kg are added in each batch.
3. The safe and efficient water reducer polyether production process according to claim 1, characterized in that: the control of the pretreatment water in the fourth step can be properly relaxed to be less than or equal to 0.08 percent, the two batches of pretreatment water produced in the test are both 0.08 percent, the dehydration temperature of the first batch (076A) is 101-102 ℃, the pressure is-0.7-0.99 barg, and the maximum dehydration temperature of the second batch (079A) is 106.2 ℃, and the pressure is-0.983 barg.
4. The safe and efficient water reducer polyether production process according to claim 1, characterized in that: the pretreatment dehydration control in the fourth step needs to start Roots for vacuum reinforcement on one hand, and can properly increase the temperature to shorten the dehydration time on the other hand, but the dehydration temperature is preferably not more than 126.2 ℃ (the current head aging temperature is 124.2-126.2 ℃).
5. The safe and efficient water reducer polyether production process according to claim 1, characterized in that: in the fourth step, in the later stage of the reaction of the reactor, the feeding amount is about 14 tons, the temperature of the reactor tends to rise, and the prior intervention is required as in the normal batch.
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Citations (6)
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| US20080161509A1 (en) * | 2005-08-30 | 2008-07-03 | Basf Se | Method for Production of Polyether Alcohols |
| CN101928392A (en) * | 2009-12-15 | 2010-12-29 | 浙江皇马科技股份有限公司 | Composite method of isopentenol polyoxyethylene ether |
| CN102898638A (en) * | 2011-07-27 | 2013-01-30 | 上海东大化学有限公司 | Polyether monomer material, and preparation method and purpose thereof |
| CN103709396A (en) * | 2013-12-26 | 2014-04-09 | 四川石达化学股份有限公司 | Dihydromyrcenol polyoxyethylene ether and synthetic method thereof |
| CN104177607A (en) * | 2014-09-01 | 2014-12-03 | 浙江永杰汽车电子有限公司 | Preparation method of high epoxyethane polyether |
| CN107522856A (en) * | 2017-08-15 | 2017-12-29 | 杭州天汇精细化工有限公司 | A kind of polyethers production technology |
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2020
- 2020-10-21 CN CN202011134305.3A patent/CN112430318A/en active Pending
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| US20080161509A1 (en) * | 2005-08-30 | 2008-07-03 | Basf Se | Method for Production of Polyether Alcohols |
| CN101928392A (en) * | 2009-12-15 | 2010-12-29 | 浙江皇马科技股份有限公司 | Composite method of isopentenol polyoxyethylene ether |
| CN102898638A (en) * | 2011-07-27 | 2013-01-30 | 上海东大化学有限公司 | Polyether monomer material, and preparation method and purpose thereof |
| CN103709396A (en) * | 2013-12-26 | 2014-04-09 | 四川石达化学股份有限公司 | Dihydromyrcenol polyoxyethylene ether and synthetic method thereof |
| CN104177607A (en) * | 2014-09-01 | 2014-12-03 | 浙江永杰汽车电子有限公司 | Preparation method of high epoxyethane polyether |
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