CN113929557A - Production method for producing trimethylolpropane by recycling carbide slag - Google Patents

Production method for producing trimethylolpropane by recycling carbide slag Download PDF

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Publication number
CN113929557A
CN113929557A CN202111166213.8A CN202111166213A CN113929557A CN 113929557 A CN113929557 A CN 113929557A CN 202111166213 A CN202111166213 A CN 202111166213A CN 113929557 A CN113929557 A CN 113929557A
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carbide slag
formaldehyde
trimethylolpropane
recycling
condensation reaction
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卞平官
王强
裴丰
周晓华
李林全
郭忠
朱露露
彭超
覃继磊
邓永兰
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Yidu Branch Of Hubei Yihua Chemical Co ltd
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Yidu Branch Of Hubei Yihua Chemical Co ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/02Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the alkali- or alkaline earth metals or beryllium
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/132Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group
    • C07C29/136Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group of >C=O containing groups, e.g. —COOH
    • C07C29/14Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group of >C=O containing groups, e.g. —COOH of a —CHO group

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  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)
  • Removal Of Specific Substances (AREA)

Abstract

The invention provides a production method for producing trimethylolpropane by recycling carbide slag, which is characterized in that calcium hydroxide solution prepared from carbide slag produced by PVC (polyvinyl chloride) preparation by an acetylene method is used as a catalyst and added into a condensation reaction for preparing trimethylolpropane by using n-butyl aldehyde and formaldehyde as raw materials. The method utilizes a large amount of calcium hydroxide solid waste carbide slag generated in PVC production by an acetylene method as a catalyst of a disproportionation method, solves the problem that the carbide slag is greatly floated by the quality of raw material carbide and process conditions, and has the difficulties of high impurity content, complex impurity types, slag removal of the carbide slag and difficult effective separation from products. Meanwhile, the wall-bonding phenomenon generated by calcium formate is easily caused by directly adding a calcium hydroxide solution as a catalyst, and the solid formed by calcium formate wall-bonding has the characteristics of strong adhesive force and compact solid, is difficult to clean, high in finished product, easy to cause equipment blockage and stop, and can not be cleaned and discarded in serious cases.

Description

Production method for producing trimethylolpropane by recycling carbide slag
Technical Field
The invention belongs to the field of chemical production, and particularly relates to a production method for producing trimethylolpropane by recycling carbide slag.
Background
Acetylene prepared by a calcium carbide method generates a large amount of calcium carbide slag waste, the calcium carbide slag waste mainly contains calcium hydroxide, impurities mainly comprise a plurality of metal oxides such as silicon, aluminum and the like, the calcium carbide slag is greatly floated when being subjected to the quality of raw calcium carbide and process working conditions, and the calcium carbide slag is high in impurity content, complex in impurity types, difficult in slag removal and difficult to effectively separate from products. In the separation of calcium formate, the wall-bonding phenomenon of calcium formate is easy to occur, and the situations of pipe blockage and too thick wall-hanging on the inner wall of equipment are easy to cause.
Disclosure of Invention
In order to solve the technical problem, the invention provides a production method for producing trimethylolpropane by recycling carbide slag.
The technical scheme adopted by the invention is as follows:
a production method for producing trimethylolpropane by recycling carbide slag is characterized in that carbide slag generated by PVC (polyvinyl chloride) preparation through an acetylene method is used as a catalyst and is added into a condensation reaction for preparing trimethylolpropane by using n-butyl aldehyde and formaldehyde as raw materials.
Preferably, the method comprises the steps of:
s1: adding an anti-saccharification auxiliary agent into the formaldehyde solution, then adding carbide slag, uniformly adding n-butyl aldehyde into the formaldehyde solution for condensation reaction according to the reaction time of 100-120 minutes, wherein the reaction temperature is 25-47 ℃;
s2: after the condensation reaction is finished, adding a crystal form finishing agent, wherein the crystal form finishing agent has the function of enabling crystal particles to be uniform and enabling the crystallization time to be uniform;
s3: adding a flocculating agent into the solution after the reaction to accelerate solid precipitation, filtering and separating solid and liquid after precipitation, and allowing the filtered clear liquid to enter the next step; filtering the filter residue containing a small amount of clear liquid again, recovering the filtrate obtained by secondary filtration, and collecting and treating the filter residue obtained by secondary filtration;
the production of producing the trimethylolpropane by recycling the carbide slag is finished.
Further preferably, in step S1, the weight ratio of the carbide slag to the deionized water is (0.2-0.5): 1, the mass ratio of the addition amount of the carbide slag to the n-butyraldehyde is (0.5-3): 1, the molar ratio of formaldehyde to n-butyraldehyde is (1-5): 1.
further preferably, in the step S1, the concentration of the formaldehyde solution is 90-150 g/L.
Further preferably, in step S2, the crystal form finishing agent is a composite silicone series.
Further preferably, in step S3, the precipitant is a compound polyacrylamide type aluminum-added precipitant for accelerating the precipitation effect, especially for large particles of carbide slag.
Further preferably, in step S1, the formose inhibitor used by the anti-saccharification auxiliary agent is one or a mixture of any two of alkali metal molybdate, alkaline earth metal molybdate, alkali metal tungstate and manganese salt, and the amount of the formose inhibitor is 1-10ppm of the mass of formaldehyde.
The invention has the beneficial effects that:
1. the invention utilizes a large amount of calcium hydroxide solid waste carbide slag generated in the production of PVC by an acetylene method, and reuses the solid waste.
2. The company utilizes a large amount of calcium hydroxide solid waste carbide slag generated in PVC production by an acetylene method as a catalyst of a disproportionation method, solves the wall bonding phenomenon generated by calcium hydroxide as a catalyst to separate calcium formate, and the solid formed by calcium formate wall bonding has the characteristics of strong adhesive force and compact solid, is difficult to clean, is high in finished product, is easy to cause equipment blockage and parking, and can not be cleaned and discarded in severe cases.
3. The addition of the saccharification inhibitor can completely inhibit the occurrence of the saccharification of the formaldehyde, so that the disproportionation reaction is smoothly carried out.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a comparison of the situation of wall hanging on the inner wall of a calcium formate bottle without and with the addition of the auxiliary agent;
FIG. 3 is a graph of the settling time of the invention without the addition of flocculant;
FIG. 4 is a comparison of the addition of an aluminum-containing precipitant in accordance with the present invention with an anionic polyacrylamide precipitant;
wherein: a size mixing tank 1, a condensation kettle 2, a precipitation filtering device 3, a secondary filtering device 4, a slag filling hopper 5 and a filtrate tank 6.
Detailed Description
The technical solutions of the present invention will be described in detail below with reference to the accompanying drawings and specific examples, but the present invention should not be construed as being limited to the implementable scope of the present invention.
Example 1
A production method for producing trimethylolpropane by recycling carbide slag is characterized in that carbide slag generated by PVC (polyvinyl chloride) preparation through an acetylene method is used as a catalyst and is added into a condensation reaction for preparing trimethylolpropane by using n-butyl aldehyde and formaldehyde as raw materials.
Preferably, the method comprises the steps of:
s1: adding an anti-saccharification auxiliary agent into the formaldehyde solution, then adding carbide slag, uniformly adding n-butyl aldehyde into the formaldehyde solution for condensation reaction according to the reaction time of 100-plus-energy for 120 minutes, wherein the reaction temperature is 30 ℃;
s2: after the condensation reaction is finished, adding a crystal form finishing agent, wherein the crystal form finishing agent has the function of enabling crystal particles to be uniform and enabling the crystallization time to be uniform;
s3: adding a flocculating agent into the solution after the reaction to accelerate solid precipitation, filtering and separating solid and liquid after precipitation, and allowing the filtered clear liquid to enter the next step; filtering the filter residue containing a small amount of clear liquid again, recovering the filtrate obtained by secondary filtration, and collecting and treating the filter residue obtained by secondary filtration;
the production of producing the trimethylolpropane by recycling the carbide slag is finished.
Further preferably, in step S1, the weight ratio of the carbide slag to the deionized water is 0.3: 1, the mass ratio of the addition amount of the carbide slag to the n-butyraldehyde is 0.4: 1, the molar ratio of formaldehyde to n-butyraldehyde is 4: 1.
further preferably, in the step S1, the concentration of the formaldehyde solution is 100 g/L.
Further preferably, in step S2, the crystal form finishing agent is a composite silicone series.
Further preferably, in step S3, the precipitant is a compound polyacrylamide type aluminum-added precipitant for accelerating the precipitation effect, especially for large particles of carbide slag.
Further preferably, in step S1, the formose inhibitor used as the anti-saccharification auxiliary agent is an alkaline earth metal molybdate, and the dosage is 6ppm of the mass of formaldehyde.
Step S1 adding anti-saccharification aid, step S2 adding crystal form finishing agent, step S3 flocculating agent (experimental conditions of example 1), versus no addition of aid control: and (3) comparing the situations of no adding of an anti-saccharification auxiliary agent in the step S1, no adding of a crystal form finishing agent in the step S2, no adding of a flocculating agent in the step S3 and wall hanging of the inner wall of the calcium formate bottle with the two auxiliary agents.
As shown in fig. 2, fig. 2a shows that calcium formate is obviously attached to the inner wall of the bottle after the condensed liquid is poured out without adding an auxiliary agent; FIG. 2b shows that the adhesion of calcium formate to the inner wall of the bottle was improved significantly after the addition of the auxiliary (conditions of example 1), and that the slight adhesion of calcium formate to the inner wall of the mouth was caused by the rapid cooling of the upper part and the lower part of the liquid surface during pouring and the rapid cooling of the calcium formate and trimethylolpropane.
Example 2
A production method for producing trimethylolpropane by recycling carbide slag is characterized in that carbide slag generated by PVC (polyvinyl chloride) preparation through an acetylene method is used as a catalyst and is added into a condensation reaction for preparing trimethylolpropane by using n-butyl aldehyde and formaldehyde as raw materials.
Preferably, the method comprises the steps of:
s1: adding an anti-saccharification auxiliary agent into the formaldehyde solution, then adding carbide slag, uniformly adding n-butyl aldehyde into the formaldehyde solution for condensation reaction according to the reaction time of 100-plus-energy for 120 minutes, wherein the reaction temperature is 30 ℃;
s2: after the condensation reaction is finished, adding a crystal form finishing agent, wherein the crystal form finishing agent has the function of enabling crystal particles to be uniform and enabling the crystallization time to be uniform;
s3: adding a flocculating agent into the solution after the reaction to accelerate solid precipitation, filtering and separating solid and liquid after precipitation, and allowing the filtered clear liquid to enter the next step; filtering the filter residue containing a small amount of clear liquid again, recovering the filtrate obtained by secondary filtration, and collecting and treating the filter residue obtained by secondary filtration;
the production of producing the trimethylolpropane by recycling the carbide slag is finished.
Further preferably, in step S1, the weight ratio of the carbide slag to the deionized water is 0.3: 1, the mass ratio of the addition amount of the carbide slag to the n-butyraldehyde is 0.4: 1, the molar ratio of formaldehyde to n-butyraldehyde is 3: 1.
further preferably, in the step S1, the concentration of the formaldehyde solution is 120 g/L.
Further preferably, in step S2, the crystal form finishing agent is a composite silicone series.
Further preferably, in step S3, the precipitant is a compound polyacrylamide type aluminum-added precipitant for accelerating the precipitation effect, especially for large particles of carbide slag.
Further preferably, in step S1, the formose inhibitor used as the anti-saccharification auxiliary agent is an alkaline earth metal molybdate, and the dosage is 6ppm of the mass of formaldehyde.
And step S1, adding the anti-saccharification auxiliary agent, and comparing the impurity content in the trimethylolpropane preliminary distillate without adding the anti-saccharification auxiliary agent.
TABLE 1
Item Trimethylolpropane content (%) Content of impurities (%)
Adding an anti-saccharification auxiliary agent 90.5 9.5
Without adding anti-saccharification auxiliary agent 85.2 14.8
As can be seen from Table 1, under the same conditions, the content of impurities in the final trimethylolpropane product is reduced by 5.3% when the anti-saccharification auxiliary agent is added or not added, which is obviously helpful for inhibiting the generation of impurities.
Example 3
A production method for producing trimethylolpropane by recycling carbide slag is characterized in that carbide slag generated by PVC (polyvinyl chloride) preparation through an acetylene method is used as a catalyst and is added into a condensation reaction for preparing trimethylolpropane by using n-butyl aldehyde and formaldehyde as raw materials.
Preferably, the method comprises the steps of:
s1: adding an anti-saccharification auxiliary agent into the formaldehyde solution, then adding carbide slag, uniformly adding n-butyl aldehyde into the formaldehyde solution for condensation reaction according to the reaction time of 100-plus-energy for 120 minutes, wherein the reaction temperature is 30 ℃;
s2: after the condensation reaction is finished, adding a crystal form finishing agent, wherein the crystal form finishing agent has the function of enabling crystal particles to be uniform and enabling the crystallization time to be uniform;
s3: adding a flocculating agent into the solution after the reaction to accelerate solid precipitation, filtering and separating solid and liquid after precipitation, and allowing the filtered clear liquid to enter the next step; filtering the filter residue containing a small amount of clear liquid again, recovering the filtrate obtained by secondary filtration, and collecting and treating the filter residue obtained by secondary filtration;
the production of producing the trimethylolpropane by recycling the carbide slag is finished.
Further preferably, in step S1, the weight ratio of the carbide slag to the deionized water is 0.3: 1, the mass ratio of the addition amount of the carbide slag to the n-butyraldehyde is 0.4: 1, the molar ratio of formaldehyde to n-butyraldehyde is 3: 1.
further preferably, in the step S1, the concentration of the formaldehyde solution is 120 g/L.
Further preferably, in step S2, the crystal form finishing agent is a composite silicone series.
Further preferably, in step S3, the precipitant is a compound polyacrylamide type aluminum-added precipitant for accelerating the precipitation effect, especially for large particles of carbide slag.
Further preferably, in step S1, the formose inhibitor used as the anti-saccharification auxiliary agent is an alkaline earth metal molybdate, and the dosage is 6ppm of the mass of formaldehyde.
The effect of adding no flocculant in step S3 was compared to the effect of adding flocculant for a 2 minute settling time.
As shown in FIG. 3, FIG. 3a shows that the solution is turbid, the precipitation effect is poor and the solution is not layered for a long time without adding a flocculating agent; FIG. 3b shows that after the flocculant is added, the solution is quickly layered in a short time, and the supernatant is clear and transparent, so that the effect is obvious.
Example 4
A production method for producing trimethylolpropane by recycling carbide slag is characterized in that carbide slag generated by PVC (polyvinyl chloride) preparation through an acetylene method is used as a catalyst and is added into a condensation reaction for preparing trimethylolpropane by using n-butyl aldehyde and formaldehyde as raw materials.
Preferably, the method comprises the steps of:
s1: adding an anti-saccharification auxiliary agent into the formaldehyde solution, then adding carbide slag, uniformly adding n-butyl aldehyde into the formaldehyde solution for condensation reaction according to the reaction time of 100-plus-energy for 120 minutes, wherein the reaction temperature is 30 ℃;
s2: after the condensation reaction is finished, adding a crystal form finishing agent, wherein the crystal form finishing agent has the function of enabling crystal particles to be uniform and enabling the crystallization time to be uniform;
s3: adding a flocculating agent into the solution after the reaction to accelerate solid precipitation, filtering and separating solid and liquid after precipitation, and allowing the filtered clear liquid to enter the next step; filtering the filter residue containing a small amount of clear liquid again, recovering the filtrate obtained by secondary filtration, and collecting and treating the filter residue obtained by secondary filtration;
the production of producing the trimethylolpropane by recycling the carbide slag is finished.
Further preferably, in step S1, the weight ratio of the carbide slag to the deionized water is 0.3: 1, the mass ratio of the addition amount of the carbide slag to the n-butyraldehyde is 0.4: 1, the molar ratio of formaldehyde to n-butyraldehyde is 3: 1.
further preferably, in the step S1, the concentration of the formaldehyde solution is 120 g/L.
Further preferably, in step S2, the crystal form finishing agent is a composite silicone series.
Further preferably, in step S3, the precipitant is a compound polyacrylamide type aluminum-added precipitant for accelerating the precipitation effect, especially for large particles of carbide slag.
Further preferably, in step S1, the formose inhibitor used as the anti-saccharification auxiliary agent is an alkaline earth metal molybdate, and the dosage is 6ppm of the mass of formaldehyde.
As shown in fig. 4, fig. 4a shows that the precipitation of the solution is good, the supernatant is clear, and the solid-liquid separation is obvious when the compound polyacrylamide precipitant with aluminum is added in step S3; FIG. 4b shows that solid and liquid can be separated by adding anionic polyacrylamide, but the effect is poor, and the supernatant is turbid.
Example 5
A production method for producing trimethylolpropane by recycling carbide slag is characterized in that carbide slag generated by PVC (polyvinyl chloride) preparation through an acetylene method is used as a catalyst and is added into a condensation reaction for preparing trimethylolpropane by using n-butyl aldehyde and formaldehyde as raw materials.
Preferably, the method comprises the steps of:
s1: adding an anti-saccharification auxiliary agent into the formaldehyde solution, then adding carbide slag, uniformly adding n-butyl aldehyde into the formaldehyde solution for condensation reaction according to the reaction time of 100-plus-energy for 120 minutes, wherein the reaction temperature is 30 ℃;
s2: after the condensation reaction is finished, adding a crystal form finishing agent, wherein the crystal form finishing agent has the function of enabling crystal particles to be uniform and enabling the crystallization time to be uniform;
s3: adding a flocculating agent into the solution after the reaction to accelerate solid precipitation, filtering and separating solid and liquid after precipitation, and allowing the filtered clear liquid to enter the next step; filtering the filter residue containing a small amount of clear liquid again, recovering the filtrate obtained by secondary filtration, and collecting and treating the filter residue obtained by secondary filtration;
the production of producing the trimethylolpropane by recycling the carbide slag is finished.
Further preferably, in step S1, the weight ratio of the carbide slag to the deionized water is 0.3: 1, the mass ratio of the addition amount of the carbide slag to the n-butyraldehyde is 0.4: 1, the molar ratio of formaldehyde to n-butyraldehyde is 3: 1.
further preferably, in the step S1, the concentration of the formaldehyde solution is 120 g/L.
Further preferably, in step S2, the crystal form finishing agent is a composite silicone series.
Further preferably, in step S3, the precipitant is a compound polyacrylamide type aluminum-added precipitant for accelerating the precipitation effect, especially for large particles of carbide slag.
Further preferably, in step S1, the formose inhibitor used as the anti-saccharification auxiliary agent is an alkaline earth metal molybdate, and the dosage is 6ppm of the mass of formaldehyde.
Under the condition of controlling the mass ratio of the carbide slag to the water to be 1:4, n-butyraldehyde is uniformly added within 100 minutes of controlling the reaction time, the concentration of bottom water (formaldehyde content) is changed, and the influence of the feeding proportion on the TMP content of the condensation liquid is changed.
TABLE 2
Figure RE-GDA0003378943710000071
From Table 2, it can be seen that the TMP content of the condensation liquid is increased under the condition that the bottom water concentration is increased by 100-; under the condition of keeping the concentration of bottom water unchanged, the feeding proportion is increased from 2:1 to 4:1, and the TMP content in the condensation liquid is increased;
example 6
A production method for producing trimethylolpropane by recycling carbide slag is characterized in that carbide slag generated by PVC (polyvinyl chloride) preparation through an acetylene method is used as a catalyst and is added into a condensation reaction for preparing trimethylolpropane by using n-butyl aldehyde and formaldehyde as raw materials.
Preferably, the method comprises the steps of:
s1: adding an anti-saccharification auxiliary agent into the formaldehyde solution, then adding carbide slag, uniformly adding n-butyl aldehyde into the formaldehyde solution for condensation reaction according to the reaction time of 100-plus-energy for 120 minutes, wherein the reaction temperature is 30 ℃;
s2: after the condensation reaction is finished, adding a crystal form finishing agent, wherein the crystal form finishing agent has the function of enabling crystal particles to be uniform and enabling the crystallization time to be uniform;
s3: adding a flocculating agent into the solution after the reaction to accelerate solid precipitation, filtering and separating solid and liquid after precipitation, and allowing the filtered clear liquid to enter the next step; filtering the filter residue containing a small amount of clear liquid again, recovering the filtrate obtained by secondary filtration, and collecting and treating the filter residue obtained by secondary filtration;
the production of producing the trimethylolpropane by recycling the carbide slag is finished.
Further preferably, in step S1, the weight ratio of the carbide slag to the deionized water is 0.3: 1, the mass ratio of the addition amount of the carbide slag to the n-butyraldehyde is 0.4: 1, the molar ratio of formaldehyde to n-butyraldehyde is 3: 1.
further preferably, in step S2, the crystal form finishing agent is a composite silicone series.
Further preferably, in step S3, the precipitant is a compound polyacrylamide type aluminum-added precipitant for accelerating the precipitation effect, especially for large particles of carbide slag.
Further preferably, in step S1, the formose inhibitor used as the anti-saccharification auxiliary agent is an alkaline earth metal molybdate, and the dosage is 6ppm of the mass of formaldehyde.
At a bottom water concentration of 120g/l, formaldehyde: the proportion of n-butyraldehyde is 3:1, and the mass ratio of carbide slag to deionized water has influence on the TMP content of the primary distillate under the condition of reaction time of 100 minutes. The mass ratio of the carbide slag to the water is best under the condition of 1: 4. The carbide slag and water are not adopted, and the mass ratio of the carbide slag to the water is 1:10, so that the water is not easy to separate, and the energy consumption is increased.
TABLE 3
Mass ratio of carbide slag to water Primary distillate TMP content (%)
1∶2 87.4
1∶3 88.2
1∶4 89.5
1∶5 89.1
1∶10 88.7
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.

Claims (7)

1. A production method for producing trimethylolpropane by recycling carbide slag is characterized in that the carbide slag generated by PVC (polyvinyl chloride) preparation by an acetylene method is used as a catalyst and is added into a condensation reaction for preparing trimethylolpropane by using n-butyl aldehyde and formaldehyde as raw materials.
2. The method for producing trimethylolpropane by recycling carbide slag according to claim 1, characterized by comprising the following steps:
s1: adding an anti-saccharification auxiliary agent into the formaldehyde solution, then adding carbide slag, uniformly adding n-butyl aldehyde into the formaldehyde solution for condensation reaction according to the reaction time of 100-120 minutes, wherein the reaction temperature is 25-47 ℃;
s2: after the condensation reaction is finished, adding a crystal form finishing agent;
s3: adding a flocculating agent into the solution after the reaction to accelerate solid precipitation, filtering and separating solid and liquid after precipitation, and allowing the filtered clear liquid to enter the next step; filtering the filter residue containing a small amount of clear liquid again, recovering the filtrate obtained by secondary filtration, and collecting and treating the filter residue obtained by secondary filtration;
the production of producing the trimethylolpropane by recycling the carbide slag is finished.
3. The method according to claim 2, wherein in step S1, the weight ratio of carbide slag to deionized water is (0.2-0.5): 1, the mass ratio of the addition amount of the carbide slag to the n-butyraldehyde is (0.5-3): 1, the molar ratio of formaldehyde to n-butyraldehyde is (1-5): 1.
4. the method as claimed in claim 2, wherein the concentration of the formaldehyde solution in step S1 is 90-150 g/L.
5. The method according to claim 2, wherein in step S2, the crystal form finishing agent is a composite silicone series.
6. The method of claim 2, wherein in step S3, the precipitant is a compound polyacrylamide type aluminum-added precipitant.
7. The method of claim 2, wherein in step S1, the formose inhibitor used in the anti-saccharification auxiliary agent is one or a mixture of any of alkali metal molybdate, alkaline earth metal molybdate, alkali metal tungstate and manganese salt, and the formose inhibitor is used in an amount of 1-10ppm based on the mass of formaldehyde.
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CN102795964B (en) * 2012-09-12 2013-05-29 江西高信有机化工有限公司 20000-ton-annual-yield production technique of trimethylolpropane by calcium method
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Application publication date: 20220114