CN115108908A - Preparation method of multi-purpose additive pentaerythritol stearate - Google Patents

Preparation method of multi-purpose additive pentaerythritol stearate Download PDF

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Publication number
CN115108908A
CN115108908A CN202210519570.6A CN202210519570A CN115108908A CN 115108908 A CN115108908 A CN 115108908A CN 202210519570 A CN202210519570 A CN 202210519570A CN 115108908 A CN115108908 A CN 115108908A
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China
Prior art keywords
pentaerythritol
pentaerythritol stearate
stearic acid
stearate
acetaldehyde
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CN202210519570.6A
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Inventor
徐昇
徐怀义
闵菊平
黄书坚
邵磊
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GUANGZHOU CARDLO BIOCHEMICAL TECHNOLOGY CO LTD
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GUANGZHOU CARDLO BIOCHEMICAL TECHNOLOGY CO LTD
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Priority to CN202210519570.6A priority Critical patent/CN115108908A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/08Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
    • 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
    • C07C29/36Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring increasing the number of carbon atoms by reactions with formation of hydroxy groups, which may occur via intermediates being derivatives of hydroxy, e.g. O-metal
    • C07C29/38Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring increasing the number of carbon atoms by reactions with formation of hydroxy groups, which may occur via intermediates being derivatives of hydroxy, e.g. O-metal by reaction with aldehydes or ketones
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention relates to a preparation method of pentaerythritol stearate, in particular to a preparation method of a multipurpose additive pentaerythritol stearate, which comprises 1 part of formaldehyde, 10 parts of acetaldehyde, 10 parts of calcium hydroxide, 1-4 parts of pentaerythritol, 20 parts of stearic acid and 0.01-0.2 part of zinc oxide; preparing pentaerythritol through appropriate amount of formaldehyde, acetaldehyde and calcium hydroxide; and step two, preparing pentaerythritol stearate from a proper amount of pentaerythritol, stearic acid and zinc oxide. The method has the advantages that the pentaerythritol is prepared by adopting a proper amount of formaldehyde, acetaldehyde and calcium hydroxide, the quality of the pentaerythritol can be improved, the condition that the cost for directly purchasing the polymer tetrol is high and the quality is uneven is avoided, the pentaerythritol is prepared by condensing, dealcoholizing, evaporating, crystallizing, filtering and drying the formaldehyde, the acetaldehyde and the calcium hydroxide according to a certain concentration, the steps of the method are simple, and the purchasing cost of pentaerythritol raw materials can be saved.

Description

Preparation method of multi-purpose additive pentaerythritol stearate
Technical Field
The invention relates to a preparation method of pentaerythritol stearate.
Background
Pentaerythritol stearate (PETS) is a white hard high melting point wax, and is dissolved in ethanol or benzene. 1, a plasticizer plays roles of plastication and lubrication in the rubber plastication process. 2. Stabilizer, processing stabilizer for polyvinyl chloride and other polymers, plasticizer and internal lubricant. 3. The lubricant is used as high-grade lubricant compounding agent and lubricant for cutting and rolling thin steel plate.
However, the pentaerythritol stearate in the prior art has low yield and low purity in the preparation method, and aiming at the problem, the preparation method of the multi-purpose additive pentaerythritol stearate is provided.
Disclosure of Invention
The invention aims to provide a preparation method of a multipurpose additive pentaerythritol stearate, which solves the problems in the background technology. In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a multipurpose additive pentaerythritol stearate comprises 1 part of formaldehyde, 10 parts of acetaldehyde, 10 parts of calcium hydroxide, 1-4 parts of pentaerythritol, 20 parts of stearic acid and 0.01-0.2 part of zinc oxide;
preparing pentaerythritol through appropriate amount of formaldehyde, acetaldehyde and calcium hydroxide;
and step two, preparing pentaerythritol stearate from a proper amount of pentaerythritol, stearic acid and zinc oxide.
Preferably, the preparation method of pentaerythritol further comprises:
condensing a proper amount of formaldehyde, acetaldehyde and calcium hydroxide according to a certain concentration to obtain a mixture A;
step two, removing aldehyde from the mixture A prepared in the step one to obtain a mixture B;
step three, putting the mixture B prepared in the step two into a container for evaporation and crystallization;
and step four, putting the powder prepared by evaporating and crystallizing the mixture B into a centrifugal machine, performing high-speed centrifugal filtration by using centrifugal force, and then performing drying treatment to obtain pure pentaerythritol.
Preferably, the condensation temperature condition of the formaldehyde, the acetaldehyde and the calcium hydroxide is 20-70 ℃, and the reaction time is 3 hours.
Preferably, the method of drying treatment comprises;
step one, placing the centrifuged wet pentaerythritol into an inner cavity of a dryer, and drying for 20min at the temperature of 100-200 ℃;
and step two, taking out the dried pentaerythritol and placing the pentaerythritol in a clean container.
Preferably, the preparation method of the pentaerythritol stearate comprises the following steps:
step one, putting a proper amount of stearic acid into an inner cavity of a reaction kettle, and heating at the temperature of 50-100 ℃ to completely melt the stearic acid;
step two, putting the completely melted stearic acid into an esterification tank, adding a proper amount of pentaerythritol and zinc oxide, and heating for 4 hours at the temperature of 120-280 ℃ to obtain a reactant;
taking out the reactant by using a sampler, and detecting the pH value of the reactant by using a pH test paper;
and step four, taking out the reactant with the pH value meeting the standard, and filtering to complete the preparation of the pentaerythritol stearate.
Preferably, the reactant has a pH of 5.
Preferably, the method of filtering comprises:
step one, connecting an input end of a drainage pump to a liquid outlet of an esterification tank, and introducing an output end of the drainage pump to a feed inlet of a filter;
starting a filter to filter the pentaerythritol stearate for 20 min;
and step three, closing the filter, and taking out the filtered pentaerythritol stearate to finish the filtration.
Preferably, the stearic acid has a quality index model of 1839 or 1838.
Compared with the prior art, the invention has the beneficial effects that:
1. the method has the advantages that the pentaerythritol is prepared by adopting a proper amount of formaldehyde, acetaldehyde and calcium hydroxide, the quality of the pentaerythritol can be improved, the condition that the cost for directly purchasing polymer tetrol is high and the quality is uneven is avoided, the pentaerythritol is prepared by condensing, dealcoholizing, evaporating, crystallizing, filtering and drying the formaldehyde, the acetaldehyde and the calcium hydroxide according to a certain concentration, the steps of the method are simple, and the purchasing cost of pentaerythritol raw materials can be saved;
2. the pentaerythritol stearate with the pH value of 5 is obtained after esterification reaction of a proper amount of pentaerythritol, stearic acid and zinc oxide, the preparation of the pentaerythritol stearate is realized, the steps and the method are simple and convenient, the preparation time of the pentaerythritol stearate can be shortened, the yield is high, the cost is low, and the investment is reduced.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
The invention provides a technical scheme that: a preparation method of a multipurpose additive pentaerythritol stearate comprises 1 part of formaldehyde, 10 parts of acetaldehyde, 10 parts of calcium hydroxide, 1 part of pentaerythritol, 20 parts of stearic acid and 0.01 part of zinc oxide;
preparing pentaerythritol by using a proper amount of formaldehyde, acetaldehyde and calcium hydroxide, and preparing pentaerythritol by using a proper amount of formaldehyde, acetaldehyde and calcium hydroxide, so that the quality of pentaerythritol can be improved, the condition that the cost of directly purchasing polymer tetrol is uneven in high quality is avoided, the pentaerythritol is prepared by condensing, dealcoholizing, evaporating, crystallizing, filtering and drying the formaldehyde, the acetaldehyde and the calcium hydroxide according to a certain concentration, the method has simple steps, and the purchasing cost of pentaerythritol raw materials can be saved;
and secondly, preparing pentaerythritol stearate from a proper amount of pentaerythritol, stearic acid and zinc oxide, and performing esterification reaction on the pentaerythritol, the stearic acid and the zinc oxide to obtain the pentaerythritol stearate with the pH value of 5.
In this embodiment, the method for preparing pentaerythritol further includes:
condensing a proper amount of formaldehyde, acetaldehyde and calcium hydroxide according to a certain concentration to obtain a mixture A, and fully reacting the formaldehyde, the acetaldehyde and the calcium hydroxide through a condensation reaction to obtain the mixture A;
step two, removing aldehyde from the mixture A prepared in the step one to obtain a mixture B;
step three, putting the mixture B prepared in the step two into a container for evaporation and crystallization;
and fourthly, putting the powder prepared by evaporating and crystallizing the mixture B into a centrifugal machine, performing high-speed centrifugal filtration by using centrifugal force, and then performing drying treatment to obtain pure pentaerythritol, wherein the pentaerythritol is prepared by filtering formaldehyde, acetaldehyde and calcium hydroxide according to a certain concentration under the centrifugal force action of the centrifugal machine, so that impurities in the pentaerythritol are filtered out, the purity of the pentaerythritol is improved, the quality of the pentaerythritol is improved, the influence on the quality of pentaerythritol stearate caused by low purity of the pentaerythritol is avoided, the impurities in the pentaerythritol are prevented from reacting with other raw materials when the pentaerythritol stearate is prepared, and the quality of the pentaerythritol is improved.
In the embodiment, the condensation temperature condition of the formaldehyde, the acetaldehyde and the calcium hydroxide is 20 ℃, the reaction time is 3 hours, the formaldehyde, the acetaldehyde and the calcium hydroxide are reacted for 3 hours at 20 ℃, the formaldehyde, the acetaldehyde and the calcium hydroxide can be fully reacted, the phenomenon that the formaldehyde, the acetaldehyde and the calcium hydroxide are not reacted completely to cause waste of raw materials is avoided, the production cost is increased, and the quality of the pentaerythritol is reduced.
In this embodiment, the method of drying includes;
putting the centrifuged wet pentaerythritol into an inner cavity of a dryer, and drying for 20min at the temperature of 100 ℃ to keep the pentaerythritol dry before esterification reaction, so as to avoid the wet pentaerythritol participating in the esterification reaction with stearic acid and causing the reduction of product quality;
and step two, taking out the dried pentaerythritol and placing the pentaerythritol in a clean container.
In this embodiment, the preparation method of pentaerythritol stearate includes:
step one, putting a proper amount of stearic acid into an inner cavity of a reaction kettle, heating at the temperature of 50 ℃ to completely melt the stearic acid, facilitating the reaction of the stearic acid and pentaerythritol, enlarging the contact area of the pentaerythritol and the stearic acid, shortening the reaction time and enabling the stearic acid and the pentaerythritol to react more thoroughly;
putting the completely melted stearic acid into an esterification tank, adding a proper amount of pentaerythritol and zinc oxide, catalyzing the reaction of the stearic acid and the pentaerythritol by adding the zinc oxide, accelerating the reaction speed of the stearic acid and the pentaerythritol, shortening the preparation time of pentaerythritol stearate, accelerating the production speed of products, and heating for 4 hours at the temperature of 120 ℃ to obtain a reactant;
taking out the reactant by using a sampler, detecting the pH value of the reactant by using a pH test paper, and knowing the reaction progress of pentaerythritol and stearic acid by detecting the pH value, wherein the pH value of pentaerythritol stearate is 5;
and step four, taking out the reactant with the pH value meeting the standard, filtering the reactant, filtering out impurities in the pentaerythritol stearate, improving the quality of the pentaerythritol stearate, and avoiding the influence on the quality of the pentaerythritol stearate due to the impurity heavily doped in the pentaerythritol stearate so as to finish the preparation of the pentaerythritol stearate.
In this embodiment, the ph of the reactant is 5, so that the reaction progress of pentaerythritol and stearic acid can be known, and the ph of pentaerythritol stearate is 5.
In this embodiment, the filtering method includes:
step one, connecting an input end of a drainage pump to a liquid outlet of an esterification tank, and introducing an output end of the drainage pump to a feed inlet of a filter;
starting a filter to filter the pentaerythritol stearate for 20 min;
and step three, closing the filter, and taking out the filtered pentaerythritol stearate to finish the filtering.
In this embodiment, the stearic acid has a quality index model of 1838.
Example 2
The invention provides a technical scheme that: a preparation method of a multipurpose additive pentaerythritol stearate comprises 1 part of formaldehyde, 10 parts of acetaldehyde, 10 parts of calcium hydroxide, 4 parts of pentaerythritol, 20 parts of stearic acid and 0.01-0.2 part of zinc oxide;
preparing pentaerythritol by using a proper amount of formaldehyde, acetaldehyde and calcium hydroxide, and preparing pentaerythritol by using a proper amount of formaldehyde, acetaldehyde and calcium hydroxide, so that the quality of pentaerythritol can be improved, the condition that the cost of directly purchasing polymer tetrol is uneven in high quality is avoided, the pentaerythritol is prepared by condensing, dealcoholizing, evaporating, crystallizing, filtering and drying the formaldehyde, the acetaldehyde and the calcium hydroxide according to a certain concentration, the method has simple steps, and the purchasing cost of pentaerythritol raw materials can be saved;
and secondly, preparing pentaerythritol stearate from a proper amount of pentaerythritol, stearic acid and zinc oxide, and performing esterification reaction on the pentaerythritol, the stearic acid and the zinc oxide to obtain the pentaerythritol stearate with the pH value of 5.
In this embodiment, the method for preparing pentaerythritol further includes:
condensing a proper amount of formaldehyde, acetaldehyde and calcium hydroxide according to a certain concentration to obtain a mixture A, and fully reacting the formaldehyde, the acetaldehyde and the calcium hydroxide through a condensation reaction to obtain a mixture A;
step two, removing aldehyde from the mixture A prepared in the step one to obtain a mixture B;
step three, putting the mixture B prepared in the step two into a container for evaporation and crystallization;
and fourthly, putting the powder prepared by evaporating and crystallizing the mixture B into a centrifugal machine, performing high-speed centrifugal filtration by using centrifugal force, and then performing drying treatment to obtain pure pentaerythritol, wherein the pentaerythritol is prepared by filtering formaldehyde, acetaldehyde and calcium hydroxide according to a certain concentration under the centrifugal force action of the centrifugal machine, so that impurities in the pentaerythritol are filtered out, the purity of the pentaerythritol is improved, the quality of the pentaerythritol is improved, the influence on the quality of pentaerythritol stearate caused by low purity of the pentaerythritol is avoided, the impurities in the pentaerythritol are prevented from reacting with other raw materials when the pentaerythritol stearate is prepared, and the quality of the pentaerythritol is improved.
In the embodiment, the condensation temperature condition of the formaldehyde, the acetaldehyde and the calcium hydroxide is 70 ℃, the reaction time is 3 hours, the formaldehyde, the acetaldehyde and the calcium hydroxide are reacted for 3 hours at 20 ℃, the formaldehyde, the acetaldehyde and the calcium hydroxide can be fully reacted, the waste of raw materials caused by incomplete reaction of the formaldehyde, the acetaldehyde and the calcium hydroxide is avoided, the production cost is increased, and the quality of the pentaerythritol is reduced.
In this embodiment, the method of drying includes;
putting the centrifuged wet pentaerythritol into an inner cavity of a dryer, and drying for 20min at the temperature of 200 ℃ to keep the pentaerythritol dry before esterification reaction, so as to avoid the wet pentaerythritol participating in the esterification reaction with stearic acid and causing the reduction of product quality;
and step two, taking out the dried pentaerythritol and placing the pentaerythritol in a clean container.
In this embodiment, the preparation method of pentaerythritol stearate includes:
step one, putting a proper amount of stearic acid into an inner cavity of a reaction kettle, heating at the temperature of 100 ℃ to completely melt the stearic acid, facilitating the reaction of the stearic acid and pentaerythritol, enlarging the contact area of the pentaerythritol and the stearic acid, shortening the reaction time and enabling the stearic acid and the pentaerythritol to react more thoroughly;
putting the completely melted stearic acid into an esterification tank, adding a proper amount of pentaerythritol and zinc oxide, catalyzing the reaction of the stearic acid and the pentaerythritol by adding the zinc oxide, accelerating the reaction speed of the stearic acid and the pentaerythritol, shortening the preparation time of pentaerythritol stearate, accelerating the production speed of products, and heating for 4 hours at the temperature of 280 ℃ to obtain a reactant;
taking out the reactant by using a sampler, detecting the pH value of the reactant by using a pH test paper, and knowing the reaction progress of pentaerythritol and stearic acid by detecting the pH value, wherein the pH value of pentaerythritol stearate is 5;
and step four, taking out the reactant with the pH value meeting the standard, filtering the reactant, filtering out impurities in the pentaerythritol stearate, improving the quality of the pentaerythritol stearate, and avoiding the influence on the quality of the pentaerythritol stearate due to the impurity heavily doped in the pentaerythritol stearate so as to finish the preparation of the pentaerythritol stearate.
In this embodiment, the ph of the reactant is 5, so that the reaction progress of pentaerythritol and stearic acid can be known, and the ph of pentaerythritol stearate is 5.
In this embodiment, the filtering method includes:
step one, connecting an input end of a drainage pump to a liquid outlet of an esterification tank, and introducing an output end of the drainage pump to a feed inlet of a filter;
starting a filter to filter the pentaerythritol stearate for 20 min;
and step three, closing the filter, and taking out the filtered pentaerythritol stearate to finish the filtering.
In this embodiment, the stearic acid has a quality index model of 1839.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and the preferred embodiments of the present invention are described in the above embodiments and the description, and are not intended to limit the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (8)

1. A preparation method of a multipurpose additive pentaerythritol stearate is characterized in that: comprises 1 portion of formaldehyde, 10 portions of acetaldehyde, 10 portions of calcium hydroxide, 1 to 4 portions of pentaerythritol, 20 portions of stearic acid and 0.01 to 0.2 portion of zinc oxide;
preparing pentaerythritol through appropriate amount of formaldehyde, acetaldehyde and calcium hydroxide;
and step two, preparing pentaerythritol stearate from a proper amount of pentaerythritol, stearic acid and zinc oxide.
2. The method for preparing pentaerythritol stearate as a multipurpose additive according to claim 1, wherein the method comprises the following steps: the preparation method of pentaerythritol also comprises the following steps:
condensing a proper amount of formaldehyde, acetaldehyde and calcium hydroxide according to a certain concentration to obtain a mixture A;
step two, removing aldehyde from the mixture A prepared in the step one to obtain a mixture B;
step three, putting the mixture B prepared in the step two into a container for evaporation and crystallization;
and step four, putting the powder prepared by evaporating and crystallizing the mixture B into a centrifugal machine, performing high-speed centrifugal filtration by using centrifugal force, and then performing drying treatment to obtain pure pentaerythritol.
3. The method for preparing pentaerythritol stearate as a multipurpose additive according to claim 2, wherein the method comprises the following steps: the condensation temperature condition of the formaldehyde, the acetaldehyde and the calcium hydroxide is 20-70 ℃, and the reaction time is 3 hours.
4. The method for preparing pentaerythritol stearate as a multipurpose additive according to claim 2, wherein the method comprises the following steps: the method for drying treatment comprises the following steps;
step one, placing the centrifuged wet pentaerythritol into an inner cavity of a dryer, and drying for 20min at the temperature of 100-200 ℃;
and step two, taking out the dried pentaerythritol and placing the pentaerythritol in a clean container.
5. The method for preparing pentaerythritol stearate as a multipurpose additive according to claim 1, wherein: the preparation method of the pentaerythritol stearate comprises the following steps:
step one, putting a proper amount of stearic acid into an inner cavity of a reaction kettle, and heating at the temperature of 50-100 ℃ to completely melt the stearic acid;
step two, putting the completely melted stearic acid into an esterification tank, adding a proper amount of pentaerythritol and zinc oxide, and heating for 4 hours at the temperature of 120-280 ℃ to obtain a reactant;
taking out the reactant by using a sampler, and detecting the pH value of the reactant by using a pH test paper;
and step four, taking out the reactant with the pH value meeting the standard, and filtering to complete the preparation of the pentaerythritol stearate.
6. The method for preparing pentaerythritol stearate as a multipurpose additive according to claim 5, wherein the method comprises the following steps: the pH value of the reactant is 5.
7. The method for preparing pentaerythritol stearate as a multipurpose additive according to claim 5, wherein: the filtering method comprises the following steps:
step one, connecting an input end of a drainage pump to a liquid outlet of an esterification tank, and introducing an output end of the drainage pump to a feed inlet of a filter;
starting a filter to filter the pentaerythritol stearate for 20 min;
and step three, closing the filter, and taking out the filtered pentaerythritol stearate to finish the filtration.
8. The method for preparing pentaerythritol stearate as a multipurpose additive according to claim 1, wherein the method comprises the following steps: the stearic acid has a quality index model of 1839 or 1838.
CN202210519570.6A 2022-05-12 2022-05-12 Preparation method of multi-purpose additive pentaerythritol stearate Pending CN115108908A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1651373A (en) * 2004-12-03 2005-08-10 王永军 Production technology of tetramethylol methane by using ealcium method
CN103880668A (en) * 2012-12-24 2014-06-25 青岛帅王油脂化学有限公司 Pentaerythritol stearate preparation technology
CN103880669A (en) * 2012-12-24 2014-06-25 青岛帅王油脂化学有限公司 Pentaerythritol stearate preparation method
CN104230660A (en) * 2014-09-27 2014-12-24 安徽金禾实业股份有限公司 Method for preparing 95 grade pentaerythritol

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1651373A (en) * 2004-12-03 2005-08-10 王永军 Production technology of tetramethylol methane by using ealcium method
CN103880668A (en) * 2012-12-24 2014-06-25 青岛帅王油脂化学有限公司 Pentaerythritol stearate preparation technology
CN103880669A (en) * 2012-12-24 2014-06-25 青岛帅王油脂化学有限公司 Pentaerythritol stearate preparation method
CN104230660A (en) * 2014-09-27 2014-12-24 安徽金禾实业股份有限公司 Method for preparing 95 grade pentaerythritol

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Application publication date: 20220927