CN113024373A - Production method of catalyst bismuth octoate for synthesizing polyurethane material - Google Patents
Production method of catalyst bismuth octoate for synthesizing polyurethane material Download PDFInfo
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- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 57
- 239000000463 material Substances 0.000 title claims abstract description 28
- 239000003054 catalyst Substances 0.000 title claims abstract description 26
- 229920002635 polyurethane Polymers 0.000 title claims abstract description 24
- 239000004814 polyurethane Substances 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 19
- OEOIWYCWCDBOPA-UHFFFAOYSA-N 6-methyl-heptanoic acid Chemical compound CC(C)CCCCC(O)=O OEOIWYCWCDBOPA-UHFFFAOYSA-N 0.000 claims abstract description 79
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 55
- 238000006243 chemical reaction Methods 0.000 claims abstract description 54
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000010438 heat treatment Methods 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 25
- 229910000014 Bismuth subcarbonate Inorganic materials 0.000 claims abstract description 17
- MGLUJXPJRXTKJM-UHFFFAOYSA-L bismuth subcarbonate Chemical compound O=[Bi]OC(=O)O[Bi]=O MGLUJXPJRXTKJM-UHFFFAOYSA-L 0.000 claims abstract description 17
- 229940036358 bismuth subcarbonate Drugs 0.000 claims abstract description 17
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims description 66
- 229940036348 bismuth carbonate Drugs 0.000 claims description 42
- GMZOPRQQINFLPQ-UHFFFAOYSA-H dibismuth;tricarbonate Chemical compound [Bi+3].[Bi+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O GMZOPRQQINFLPQ-UHFFFAOYSA-H 0.000 claims description 42
- 239000007788 liquid Substances 0.000 claims description 28
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims description 28
- 239000012071 phase Substances 0.000 claims description 27
- 239000011541 reaction mixture Substances 0.000 claims description 21
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 17
- 239000000376 reactant Substances 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 12
- 238000000926 separation method Methods 0.000 claims description 10
- 239000007795 chemical reaction product Substances 0.000 claims description 8
- OBETXYAYXDNJHR-UHFFFAOYSA-N alpha-ethylcaproic acid Natural products CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 claims description 7
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 7
- 125000004432 carbon atom Chemical group C* 0.000 claims description 6
- 239000012074 organic phase Substances 0.000 claims description 6
- OBETXYAYXDNJHR-SSDOTTSWSA-M (2r)-2-ethylhexanoate Chemical compound CCCC[C@@H](CC)C([O-])=O OBETXYAYXDNJHR-SSDOTTSWSA-M 0.000 claims description 4
- 239000001569 carbon dioxide Substances 0.000 claims description 4
- 230000002209 hydrophobic effect Effects 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 239000002699 waste material Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 2
- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000005580 one pot reaction Methods 0.000 abstract description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 6
- 239000008213 purified water Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- WWZKQHOCKIZLMA-UHFFFAOYSA-M octanoate Chemical compound CCCCCCCC([O-])=O WWZKQHOCKIZLMA-UHFFFAOYSA-M 0.000 description 2
- 229960002446 octanoic acid Drugs 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- -1 medical treatment Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/16—Catalysts
- C08G18/22—Catalysts containing metal compounds
- C08G18/227—Catalysts containing metal compounds of antimony, bismuth or arsenic
Abstract
The invention discloses a production method of a catalyst bismuth octoate for synthesizing a polyurethane material, which comprises the following steps: the method comprises the following steps: firstly, a user adds water into a reaction kettle, then, a heating device is used for heating the water in the reaction kettle until the water is heated to a proper temperature, and then, the user adds isooctanoic acid into the reaction kettle again, wherein the mass ratio of the water to the isooctanoic acid is 1-5: 1; according to the invention, through the cooperation of the first step, the second step, the third step, the fourth step and the fifth step, a user prepares the bismuth isooctanoate by utilizing the one-step reaction of the bismuth subcarbonate and the isooctanoic acid, the preparation process of the bismuth isooctanoate is simple and short in working procedure, and does not need to use a catalyst, so that the production cost for preparing the bismuth isooctanoate is relatively low, the industrialization is easy to realize, the development of an environment-friendly polyurethane material can be promoted, and the problems that the traditional preparation process of the bismuth isooctanoate is long in working procedure, complex in equipment, high in energy consumption, not environment-friendly or needs to use a catalyst which.
Description
Technical Field
The invention relates to the technical field of polyurethane materials, in particular to a production method of a catalyst bismuth octoate for synthesizing a polyurethane material.
Background
The polyurethane material is a novel organic polymer material, is known as the fifth plastic and is widely applied to the fields of light industry, chemical industry, electronics, textile, medical treatment, building materials, automobiles, national defense, aviation, aerospace and the like due to excellent performance, and is prepared by condensing isocyanate and oligomer polyol and adding a chain extension crosslinking agent, a flame retardant, an antioxidant, an ultraviolet absorbent, a coloring agent and a plasticizer.
Bismuth isooctanoate is a novel catalyst developed in recent years for synthesizing polyurethane materials, and the existing bismuth isooctanoate preparation process has the defects of long process, complex equipment, high energy consumption, environmental pollution or the need of using a catalyst which is difficult to obtain in the synthesis process, so that the production cost of bismuth isooctanoate is increased, the use of bismuth isooctanoate for replacing organic lead, tin and mercury catalysts is inhibited, and the popularization and the application of the environment-friendly polyurethane materials are not facilitated.
Therefore, it is desirable to design a method for producing bismuth octoate used as a catalyst for synthesizing polyurethane materials to solve the above problems.
Disclosure of Invention
The invention aims to provide a production method of a catalyst bismuth octoate for synthesizing a polyurethane material, and aims to solve the problems that the traditional bismuth isooctanoate preparation process proposed in the background technology has long working procedures, complicated equipment, high energy consumption, no environmental protection or the need of using a catalyst which is difficult to obtain in the synthesis process and the like.
In order to achieve the purpose, the invention provides the following technical scheme: a production method of a catalyst bismuth octoate for synthesizing a polyurethane material comprises the following steps:
the method comprises the following steps: firstly, a user adds water into a reaction kettle, then, a heating device is used for heating the water in the reaction kettle until the water is heated to a proper temperature, and then, the user adds isooctanoic acid into the reaction kettle again, wherein the mass ratio of the water to the isooctanoic acid is 1-5: 1;
step two: after adding water and isooctanoic acid, a user utilizes a stirring rod to stir the raw materials for 10-30 minutes, then basic bismuth carbonate is added into a reaction kettle, wherein the molar ratio of the added basic bismuth carbonate to the basic bismuth carbonate is 6.05-6.1: 1, and slight excess of isooctanoic acid is always kept;
step three: with the addition of the basic bismuth carbonate, the color of the reaction mixture is slowly changed from white to light yellow and yellow, and finally to yellow with brown, after the basic bismuth carbonate is completely added, a user continuously utilizes the stirring rod to heat and stir the basic bismuth carbonate, and after the stirring is finished, the power supply is turned off, and meanwhile, the heating and the stirring of the reaction mixture are stopped;
step four: then, the reaction mixture is prevented from standing aside, after a period of time, the reaction product stands until the solution is divided into an upper phase and a lower phase, the lower phase is an organic phase bismuth octoate which has high density and is tawny oleophylic and hydrophobic, and the upper layer is a colorless, transparent, hydrophilic and oleophobic water phase with low density;
step five: and finally, separating the two phases by adopting a liquid separation method to obtain a yellow brown semitransparent bismuth isooctanoate liquid, wherein the chemical reaction formula is as follows:
6C8H15O2+(Bi)2CO3.1/2H2O＝2(C8H14O2)3Bi+CO2+7/2H20。
preferably, in the first step, when the heating device heats the water in the reaction kettle, the user uses the stirring rod to stir the water, and the temperature range for stirring and heating the water is between 65 ℃ and 95 ℃.
Preferably, during step one, the carbon atoms of the isooctanoic acid and the n-octanoic acid added into the reaction kettle are the same, and the isooctanoic acid is 2-ethyl hexanoic acid with a branch.
Preferably, during the second step, when the bismuth subcarbonate is added, a user carefully observes the reaction phenomenon, controls the adding speed of the bismuth subcarbonate according to the generated gas quantity, and adopts a method of adding the bismuth subcarbonate in batches while stirring.
Preferably, in the second step, after the isooctanoic acid and the bismuth subcarbonate are added in sequence in the reaction kettle, according to the table of acidity coefficients, the acidity coefficient pKa of the octanoic acid is 4.85, and the acidity coefficient pKa of the carbonic acid is 6.38.
Preferably, during the third step, when the user stirs the reaction mixture, the stirring time of the reactants is controlled to be 30-60 minutes according to the ratio of the reactants added.
Preferably, in the fifth step, after the yellowish-brown semitransparent bismuth isooctanoate liquid is obtained, a user can add an organic solvent to dilute the yellowish-brown semitransparent bismuth isooctanoate liquid according to actual requirements, so that yellowish transparent bismuth isooctanoate liquid with different concentrations can be obtained.
Preferably, in the fifth step, no three wastes are discharged from the reaction system in the whole process from the preparation of the reaction solution from the dissolved materials to the end of the reaction, at this time, isooctanoic acid with purity of 99.5% reacts with analytically pure alkali type bismuth carbonate, the product bismuth isooctanoate is needed, a small amount of carbon dioxide also overflows, and finally, water remains, at this time, the impurities brought in the reactants are few.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the production method of the catalyst bismuth octoate for synthesizing the polyurethane material, through the matching of the first step, the second step, the third step, the fourth step and the fifth step, a user utilizes the basic bismuth carbonate to react with the isooctanoic acid in one step to prepare the bismuth isocaprylate, and simultaneously adopts a liquid separation method to separate an organic phase from a water phase, so that the commercial bismuth isocaprylate can be obtained.
2. According to the production method of the catalyst bismuth octoate for synthesizing the polyurethane material, the temperature range of water stirring and heating is 65-95 ℃, the water temperature is controlled to be 65-95 ℃, the subsequent addition of isooctanoic acid can be ensured to be fully reacted with water, so that the reaction efficiency of isooctanoic acid and water is further improved, the carbon atom numbers of isooctanoic acid and n-octanoic acid are the same, the isooctanoic acid is a branched chain of 2-ethylhexanoic acid, and the theory is explained according to the acidity of organic acid: the method has the advantages that the carbon atoms are the same, the branched chain is multiple, the acidity is strong, the acidity of isooctanoic acid is stronger than that of n-octanoic acid, so that isooctanoic acid can be more easily reacted with carbonate to prepare isooctanoate, the isooctanoate is prepared by a method of adding the isooctanoate in batches while stirring, the added reactants can be effectively prevented from overflowing out of a reaction kettle in the reaction process, so that the added basic bismuth carbonate can be efficiently reacted with water and isooctanoic acid, the acidity coefficient pKa of n-octanoic acid is 4.85, the acidity coefficient pKa of carbonic acid is 6.38, and the theory of acidity is explained: the smaller the acidity coefficient is, the stronger the acidity is, the larger the acidity coefficient is, the weaker the acidity is, and obviously, the acidity of the n-octanoic acid is stronger than that of carbonic acid, so that the n-octanoic acid can react with the carbonate to decompose the carbonate to prepare the octanoate, the stirring time of the reactants is controlled to be 30-60 minutes according to the proportion of the reactants, and the influence on the reaction effect of the reactants due to the over-short or over-long stirring time is avoided, so that the reactants can be effectively and fully mixed, a user can dilute the reactants by adding an organic solvent according to actual requirements, and then light yellow transparent bismuth isocaprylate liquid with different concentrations can be obtained, the subsequent flexible use of the bismuth isocaprylate liquid by the user is facilitated, the preparation speed of the bismuth isocaprylate is further accelerated, no three wastes are discharged out of a reaction system in the whole process from the preparation of a dissolved material to, meanwhile, the clean water is remained, so that the secondary water recycling of the water is facilitated, and the preparation method of the bismuth isooctanoate is more environment-friendly.
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 embodiment provided by the invention comprises the following steps: a production method of a catalyst bismuth octoate for synthesizing a polyurethane material comprises the following steps:
the method comprises the following steps: firstly, a user adds water into a reaction kettle, then, a heating device is used for heating the water in the reaction kettle until the water is heated to a proper temperature, and then, the user adds isooctanoic acid into the reaction kettle again, wherein the mass ratio of the water to the isooctanoic acid is 1-5: 1;
step two: after adding water and isooctanoic acid, a user utilizes a stirring rod to stir the raw materials for 10-30 minutes, then basic bismuth carbonate is added into a reaction kettle, wherein the molar ratio of the added basic bismuth carbonate to the basic bismuth carbonate is 6.05-6.1: 1, and slight excess of isooctanoic acid is always kept;
step three: with the addition of the basic bismuth carbonate, the color of the reaction mixture is slowly changed from white to light yellow and yellow, and finally to yellow with brown, after the basic bismuth carbonate is completely added, a user continuously utilizes the stirring rod to heat and stir the basic bismuth carbonate, and after the stirring is finished, the power supply is turned off, and meanwhile, the heating and the stirring of the reaction mixture are stopped;
step four: then, the reaction mixture is prevented from standing aside, after a period of time, the reaction product stands until the solution is divided into an upper phase and a lower phase, the lower phase is an organic phase bismuth octoate which has high density and is tawny oleophylic and hydrophobic, and the upper layer is a colorless, transparent, hydrophilic and oleophobic water phase with low density;
step five: and finally, separating the two phases by adopting a liquid separation method to obtain a yellow brown semitransparent bismuth isooctanoate liquid, wherein the chemical reaction formula is as follows:
6C8H15O2+(Bi)2CO3.1/2H2O＝2(C8H14O2)3Bi+CO2+7/2H20, through the matching of the first step, the second step, the third step, the fourth step and the fifth step, a user prepares bismuth isooctanoate by using bismuth subcarbonate and isooctanoic acid through one-step reaction, and simultaneously adopts a liquid separation method to separate an organic phase and a water phase to obtain the commercial bismuth isooctanoateThe catalyst is used, so that the production cost for preparing the bismuth isooctanoate is relatively low, the industrialization is easy to realize, the development of an environment-friendly polyurethane material can be promoted, and the problems of long working procedures, complex equipment, high energy consumption, environmental pollution or the need of using a catalyst which is difficult to obtain in the synthesis process and the like in the traditional bismuth isooctanoate preparation process are solved.
In the first step of process, when heating device is heating the water in the reation kettle, the user utilizes the stirring rod to stir water this moment, and the temperature interval of stirring the water heating is between 65 ~ 95 ℃, and the temperature control can guarantee that the isooctanoic acid of follow-up joining can carry out abundant reaction with water between 65 ~ 95 ℃ to the reaction efficiency of isooctanoic acid and water has further been promoted.
In the process of the first step, the carbon atoms of the isooctanoic acid and the n-octanoic acid added into the reaction kettle are the same, the isooctanoic acid is 2-ethylhexanoic acid with a branched chain, and the theory is explained according to the acidity of organic acid: the iso-caprylic acid salt is easier to react with carbonate to prepare the iso-caprylic acid salt because the iso-caprylic acid has stronger acidity than the n-caprylic acid due to the fact that the number of carbon atoms is the same and the number of branched chains is large.
In the second step, when the bismuth subcarbonate is added, a user carefully observes the reaction phenomenon, controls the adding speed of the bismuth subcarbonate according to the generated gas quantity, and adopts a method of adding the bismuth subcarbonate in batches while stirring to prepare the bismuth subcarbonate, so that the added bismuth subcarbonate can be effectively prevented from overflowing out of the reaction kettle in the reaction process, and the added bismuth subcarbonate can be subjected to high-efficiency reaction with water and isooctanoic acid.
In the second step, after the isooctanoic acid and the bismuth subcarbonate are added into the reaction kettle in sequence, according to a table for looking up the acidity coefficient, wherein the acidity coefficient pKa of the octanoic acid is 4.85, the acidity coefficient pKa of the carbonic acid is 6.38, the theory of acidity is explained as follows: the smaller the acidity coefficient, the more acidic and the weaker the acidity coefficient, and it is obvious that n-octanoic acid is more acidic than carbonic acid, so that n-octanoic acid can react with carbonate to decompose carbonate to prepare octanoate.
In the third step, when a user stirs the reaction mixture, the stirring time of the reactants is controlled to be 30-60 minutes according to the proportion of the reactants, so that the reaction effect of the reactants is prevented from being influenced by too short or too long stirring time, and the reactants can be effectively fully mixed.
In the fifth step, after the yellowish-brown semitransparent bismuth isooctanoate liquid is obtained, a user can add an organic solvent for dilution according to actual requirements, so that the yellowish transparent bismuth isooctanoate liquid with different concentrations can be obtained, the user can use the bismuth isooctanoate liquid flexibly and conveniently, and the preparation speed of the bismuth isooctanoate is further increased.
In the fifth step, no three wastes are discharged from the reaction system in the whole process from the preparation of the reaction solution by the dissolved materials to the end of the reaction, at the moment, isooctanoic acid with the purity of 99.5% reacts with the analytical soda type bismuth carbonate, the product bismuth isooctanoate is needed, a small amount of carbon dioxide overflows at the same time, water is left, impurities brought in reactants are few, the overflow of a small amount of carbon dioxide cannot pollute the environment, clean water is remained, secondary water recycling of the water is facilitated, and therefore the preparation method of the bismuth isooctanoate is more environment-friendly.
The invention also has the following further embodiments:
example 1
Adding 80g of purified water into a reaction kettle, heating to 70 ℃ under stirring, adding 20g of isooctanoic acid, stirring for 15 minutes, adding 12g of basic bismuth carbonate in batches under stirring, gradually changing the color of a reaction mixture from white to light yellow and yellow along with the addition of the basic bismuth carbonate, finally changing the reaction mixture to yellow and brown, continuing heating and stirring for 35 minutes after the addition of the basic bismuth carbonate is finished, turning off a power supply, stopping heating and stirring, standing the reaction product until the solution is divided into two phases, wherein the lower layer is a yellowish brown oleophilic hydrophobic organic phase bismuth octoate with large density, the upper layer is a colorless transparent hydrophilic oleophobic aqueous phase with small density, separating the two phases by adopting a liquid separation method to obtain 29g of oily liquid, and the yield is 98.2 percent based on the basic bismuth carbonate.
Example 2
Adding 75g of purified water into a reaction kettle, heating to 90 ℃ under stirring, adding 75g of isooctanoic acid, stirring for 30 minutes, adding 44.6g of basic bismuth carbonate in batches under stirring, gradually changing the color of a reaction mixture from white to light yellow and yellow along with the addition of the basic bismuth carbonate, finally changing the color of the reaction mixture to be yellow and brown, continuing heating and stirring for 50 minutes after the addition of the basic bismuth carbonate is finished, turning off a power supply to stop heating and stirring, standing a reaction product until the solution is divided into two phases, separating the two phases by a liquid separation method to obtain 108.8g of oily liquid, wherein the yield is 99.12 percent calculated by the basic bismuth carbonate.
Example 3
Adding 780g of purified water into a reaction kettle, heating to 95 ℃ under stirring, adding 260g of isooctanoic acid, stirring for 25 minutes, adding 153.4g of basic bismuth carbonate while stirring in batches, gradually changing the color of a reaction mixture from white to light yellow and yellow along with the addition of the basic bismuth carbonate, finally changing the color of the reaction mixture to be yellow and brown, continuing heating and stirring for 45 minutes after the addition of the basic bismuth carbonate is finished, turning off a power supply to stop heating and stirring, standing a reaction product until the solution is divided into two phases, separating the two phases by a liquid separation method to obtain 375.4g of oily liquid, wherein the yield is 99.44 percent calculated by the basic bismuth carbonate.
Example 4
Adding 840g of purified water into a reaction kettle, heating to 85 ℃ under stirring, adding 420g of isooctanoic acid, stirring for 20 minutes, adding 250.68g of basic bismuth carbonate while stirring in batches, gradually changing the color of a reaction mixture from white to light yellow and yellow along with the addition of the basic bismuth carbonate, finally changing the color of the reaction mixture to be yellow and brown, continuing heating and stirring for 40 minutes after the addition of the basic bismuth carbonate is finished, turning off a power supply, stopping heating and stirring, standing a reaction product until the solution is divided into two phases, separating the two phases by a liquid separation method to obtain 615g of oily liquid, wherein the yield is 99.69 percent calculated by the basic bismuth carbonate.
Example 5
5500g of purified water is added into a reaction kettle, the temperature is raised to 65 ℃ under stirring, 1100g of isooctanoic acid is added, the stirring is carried out for 28 minutes, 655.46g of basic bismuth carbonate is added in batches under the stirring, the color of a reaction mixture slowly changes from white to light yellow and yellow along with the addition of the basic bismuth carbonate, and finally changes to yellow and brown, after the addition of the basic bismuth carbonate is finished, the heating and the stirring are continuously carried out for 60 minutes, the power supply is turned off to stop the heating and the stirring, the reaction product is kept stand until the solution is divided into two phases, the two phases are separated by adopting a liquid separation method to obtain 1610.2g of oily liquid, and the yield is. It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (8)
1. A production method of a catalyst bismuth octoate used for synthesizing polyurethane materials is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: firstly, a user adds water into a reaction kettle, then, a heating device is used for heating the water in the reaction kettle until the water is heated to a proper temperature, and then, the user adds isooctanoic acid into the reaction kettle again, wherein the mass ratio of the water to the isooctanoic acid is 1-5: 1;
step two: after adding water and isooctanoic acid, a user utilizes a stirring rod to stir the raw materials for 10-30 minutes, then basic bismuth carbonate is added into a reaction kettle, wherein the molar ratio of the added basic bismuth carbonate to the basic bismuth carbonate is 6.05-6.1: 1, and slight excess of isooctanoic acid is always kept;
step three: with the addition of the basic bismuth carbonate, the color of the reaction mixture is slowly changed from white to light yellow and yellow, and finally to yellow with brown, after the basic bismuth carbonate is completely added, a user continuously utilizes the stirring rod to heat and stir the basic bismuth carbonate, and after the stirring is finished, the power supply is turned off, and meanwhile, the heating and the stirring of the reaction mixture are stopped;
step four: then, the reaction mixture is prevented from standing aside, after a period of time, the reaction product stands until the solution is divided into an upper phase and a lower phase, the lower phase is an organic phase bismuth octoate which has high density and is tawny oleophylic and hydrophobic, and the upper layer is a colorless, transparent, hydrophilic and oleophobic water phase with low density;
step five: and finally, separating the two phases by adopting a liquid separation method to obtain a yellow brown semitransparent bismuth isooctanoate liquid, wherein the chemical reaction formula is as follows:
6C8H15O2+(Bi)2CO3.1/2H2O＝2(C8H14O2)3Bi+CO2+7/2H20。
2. the method for producing a catalyst bismuth octoate for synthesizing a polyurethane material according to claim 1, wherein: in the first step, when the heating device heats the water in the reaction kettle, a user utilizes the stirring rod to stir the water, and the temperature range for stirring and heating the water is between 65 and 95 ℃.
3. The method for producing a catalyst bismuth octoate for synthesizing a polyurethane material according to claim 1, wherein: in the process of the first step, the carbon atoms of the isooctanoic acid and the n-octanoic acid added into the reaction kettle are the same, and the isooctanoic acid is 2-ethylhexanoic acid with a branched chain.
4. The method for producing a catalyst bismuth octoate for synthesizing a polyurethane material according to claim 1, wherein: and in the second step, when the bismuth subcarbonate is added, a user carefully observes the reaction phenomenon, controls the adding speed of the bismuth subcarbonate according to the generated gas quantity, and adopts a method of adding the bismuth subcarbonate in batches while stirring.
5. The method for producing a catalyst bismuth octoate for synthesizing a polyurethane material according to claim 1, wherein: in the second step, after the isooctanoic acid and the bismuth subcarbonate are sequentially added into the reaction kettle, according to a table for looking up the acidity coefficient, the acidity coefficient pKa of the octanoic acid is 4.85, and the acidity coefficient pKa of the carbonic acid is 6.38.
6. The method for producing a catalyst bismuth octoate for synthesizing a polyurethane material according to claim 1, wherein: and in the third step, when a user stirs the reaction mixture, controlling the stirring time of the reactants to be 30-60 minutes according to the proportion of the reactants.
7. The method for producing a catalyst bismuth octoate for synthesizing a polyurethane material according to claim 1, wherein: in the fifth step, after the yellowish-brown semitransparent bismuth isooctanoate liquid is obtained, a user can add an organic solvent for dilution according to actual requirements, and then yellowish transparent bismuth isooctanoate liquid with different concentrations can be obtained.
8. The method for producing a catalyst bismuth octoate for synthesizing a polyurethane material according to claim 1, wherein: in the fifth step, no three wastes are discharged from the reaction system in the whole process from the preparation of the reaction solution by the dissolved materials to the end of the reaction, at this time, isooctanoic acid with the purity of 99.5% reacts with the analytical soda type bismuth carbonate, the product bismuth isooctanoate is needed, a small amount of carbon dioxide overflows, and finally, water is left, and at this time, impurities brought in the reactants are few.
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