Bis-trihydroxy material and colored impurity removal method thereof

Abstract

The invention discloses a bis-trihydroxy material and a colored impurity removal method thereof, and belongs to the field of purification and impurity removal of organic compounds, the impurity removal method comprises the following steps: adding a heavy component and a solvent into a preparation tank, stirring, adding a mother solution and deionized water, preparing, uniformly stirring, heating to 80-85 DEG C, and standing for 30 minutes to obtain a mixed material; feeding the mixed material into a separator to separate a water phase and an oil phase, and washing the oil phase with water to obtain an extracted water phase product; heating and concentrating the extracted water-phase product to remove 40% of water in the water-phase product; feeding the concentrated water-phase product into an activated carbon preparation tank for decoloration, stirring for 30 minutes at 60 DEG C, adding phosphoric acid for hydrolysis, and adjusting the pH value to 3.0-3.5 at the same time; and filtering the concentrated solution subjected to hydrolysis and color removal, cooling and crystallizing to prepare the bis-trihydroxy material. The method for removing the colored impurities is simple in process and easy to implement on a device.

Description

Technical Field

[0001] The invention relates to the technical field of purification and impurity removal of organic compounds, and in particular to a ditrihydroxy material and a method for removing colored impurities thereof. Background Art

[0002] Ditrimethylolpropane (Di-TMP, CAS No. 23235-61-2) is a planar molecule with four relatively active primary hydroxyl groups. It has superior properties than trimethylolpropane and can replace polyols such as glycerol, neopentyl glycol, pentaerythritol, trimethylolpropane, etc. It is used in the production of alkyd resins, polyurethane resins, lubricants, explosives, plasticizers, rosin esters and advanced aviation lubricants. It has unique properties in the application of surfactants and aviation lubricants. Ditrimethylolpropane is also a raw material for the production of acrylic monomers / oligomers, synthetic lubricants, special resins and chemical intermediates, coating resins, PVC stabilizers and other fine chemicals.

[0003] Ditrimethylolpropane is generally extracted as a by-product in the production process of trimethylolpropane. From the beginning of feeding, it generally needs to go through condensation reaction, evaporation, extraction, solvent recovery, distillation and other steps to obtain the heavy components that can be used to extract ditrimethylolpropane. Then, ditrimethylolpropane is extracted by distilling the extracted trimethylolpropane heavy components. Generally, the method is to first dissolve Summary of the invention

[0004] One of the purposes of the present invention is to provide a method for removing colored impurities from a ditrihydroxy material, so as to solve the disadvantage of the prior art that it is difficult to remove colored impurities from a ditrihydroxy material.

[0005] The present invention is achieved through the following technical scheme, a method for removing colored impurities from a ditrihydroxy material, comprising: S100, placing a heavy component and a solvent into a preparation tank for stirring, then adding a mother liquor and deionized water for preparation, stirring evenly and heating to 80-85°C, and standing for 30 minutes to obtain a mixed material; S200, sending the mixed material into a separator to separate an aqueous phase and an oil phase, and washing the oil phase with water to obtain an extracted aqueous phase product; S300, heating and concentrating the extracted aqueous phase product to concentrate 40% of the water in the aqueous phase product; S400, the concentrated aqueous phase product enters an activated carbon preparation tank for decolorization, stirring at 60°C for 30 minutes and adding an appropriate amount of phosphoric acid for hydrolysis, while adjusting the pH value to 3.0-3.5; S500, filtering the decolorized concentrated liquid, cooling and crystallizing it, to prepare the ditrihydroxy material.

[0006] Furthermore, in step S100, the mass ratio of the heavy component to the solvent is 1:1, and the mixture is mixed and stirred for 15 minutes before adding the mother liquor and water. The addition ratio of the mother liquor is 5 times that of the heavy component, and the addition ratio of the deionized water is 2 times that of the heavy component.

[0007] Furthermore, the solvent in step S100 is isooctyl alcohol.

[0008] Furthermore, the separator in step S200 is a separation tower, the mixed material enters the separation tower from the middle, and the water washing temperature is 90°C.

[0009] Furthermore, the temperature of the heating and concentration in step S300 is 98-102°C.

[0010] Furthermore, the amount of activated carbon added to the activated carbon preparation tank in step S400 is 0.3% of the total mass of the concentrated aqueous phase product.

[0011] Furthermore, the amount of phosphoric acid added in step S400 is 0.3-0.5% of the total mass of the concentrated aqueous phase product, and the hydrolysis time is 1 hour.

[0012] Another aspect of the present invention provides a ditrihydroxy material, which is prepared according to the above method. In the material, the wet color of the ditrihydroxy material crystal is less than 30, ditrimethylolpropane is ≥98%, and impurities are less than 2%.

[0013] Compared with the prior art, the present invention has the following advantages and beneficial effects:

[0014] The colored impurity removal method of the present invention has a simple process and is easy to implement on a device. Through configuration adjustment, system water washing, decolorization and hydrolysis and other treatments, the colored impurities in the system can be effectively removed, the chromaticity of ditrimethylolpropane can be reduced, the content of ditrimethylolpropane can be increased, and the output of the system can be effectively increased, and the recycling of heavy components can be improved, thereby achieving the effects of energy saving, emission reduction, and environmental protection. DETAILED DESCRIPTION

[0015] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments.

[0016] Unless otherwise specified, all technical and scientific terms used herein have the same meanings as commonly understood by those skilled in the art in the art of the present invention. Although the present invention describes only preferred methods and materials, any methods and materials similar or equivalent to those described herein may also be used in the implementation or testing of the present invention. All documents mentioned in this specification are incorporated by reference to disclose and describe methods and / or materials related to the documents. In the event of a conflict with any incorporated document, the content of this specification shall prevail. Regarding the "comprising", "including", "having", "containing" and the like used herein, they are all open-ended terms, that is, they mean including but not limited to. Unless the context clearly indicates otherwise, the expressions "a" and "one" used herein include plural references. The term "about" used herein means a range of ±20% of the value thereafter. In some embodiments, the term "about" means a range of ±10% of the value thereafter. In some embodiments, the term "about" means a range of ±5% of the value thereafter.

[0017] Embodiment 1,

[0018] This embodiment provides a method for removing colored impurities from a ditrihydroxy material, which can effectively remove colored impurities from the ditrihydroxy material, and can obtain a ditrihydroxy material with a chromaticity of a crystallized wet material of less than 30, ditrimethylolpropane ≥ 98%, and impurities of less than 2%. This embodiment specifically includes the following steps:

[0019] Step 1: Put the heavy component and the solvent into the preparation tank, stir, add the mother liquor and deionized water for preparation, stir evenly and heat to 80°C, and let it stand for 30 minutes to obtain a mixed material.

[0020] Specifically, the solvent is isooctyl alcohol, the mass ratio of the heavy component to the solvent is 1:1, the mixture is mixed and stirred for 15 minutes, and then the mother liquor and deionized water are added. The addition ratio of the mother liquor is 5 times that of the heavy component, and the addition ratio of the deionized water is 2 times that of the heavy component.

[0021] It should be noted that in this embodiment, the heavy components generally refer to the main organic compounds or chemical components involved in the reaction, especially in the process of removing colored impurities, these heavy components are target chemical substances that need to be separated or purified from impurities. Specifically, the heavy components can be organic molecules containing multiple hydroxyl (-OH) functional groups, or some raw materials that can be converted into useful products through chemical treatment.

[0022] Specifically, the recombinant fraction in this example is ditrimethylolpropane among the unpurified trihydroxy compounds.

[0023] Step 2: The mixed material is sent to a separation tower to separate the water phase and the oil phase, and the water washing temperature is set to 90°C to wash the oil phase with water to obtain an extracted water phase product.

[0024] Step 3: The extracted aqueous phase product is heated and concentrated at a temperature of 98° C. to concentrate 40% of the water in the aqueous phase product.

[0025] Step 4: Add 0.3% of the total mass of the concentrated aqueous product to the activated carbon preparation tank, put the concentrated aqueous product into the activated carbon preparation tank for decolorization, stir at 60°C for 30 minutes, add 0.3% of phosphoric acid to hydrolyze, and adjust the pH value to 3.0. Bistrihydroxy material.

[0026] Step 5: Filter the concentrated solution after hydrolysis and decolorization, cool and crystallize, and finally prepare a ditrihydroxy material with impurities less than 2%.

[0027] Embodiment 2,

[0028] Take 200 ml of the heavy component and prepare it according to the ratio of heavy component: solvent: mother liquor: water 1:1:5:2. Stir evenly and heat to 82°C, and let it stand for half an hour.

[0029] The prepared raw material solution, solvent, mother liquor and water enter the separation system to separate the water phase and the oil phase, and the oil phase is further washed with water.

[0030] The aqueous phase after extraction was heated and concentrated to remove 40% of the water.

[0031] The concentrated water phase enters activated carbon for decolorization. The amount of activated carbon added is 0.3% of the total mass and stirred for half an hour.

[0032] The concentrated solution after hydrolysis and decolorization is filtered, cooled and crystallized, and the wet crystals are taken for gas chromatography detection.

[0033] Embodiment 3,

[0034] Take 200 ml of the heavy component and prepare it according to the ratio of heavy component: solvent: mother liquor: water 1:1:5:2. Stir evenly and heat to 85°C, and let it stand for half an hour.

[0035] The prepared raw material solution, solvent, mother liquor and water enter the separation system to separate the water phase and the oil phase, and the oil phase is further washed with water.

[0036] The aqueous phase after extraction was heated and concentrated to remove 40% of the water.

[0037] Phosphoric acid is added for hydrolysis, and the amount of phosphoric acid added is 0.5% of the weight to ensure that the pH value of the concentrate is between 3.5.

[0038] The concentrated solution after hydrolysis and decolorization is filtered, cooled and crystallized, and the wet crystals are taken for gas chromatography detection.

[0039] Experimental example

[0040] The products prepared in Examples 1, 2 and 3 were subjected to detailed experiments, and the relevant data were shown in Table 1 below.

[0041] Table 1.

[0042]

[0043] From the results in the above table, it can be seen that after treatment, the chromaticity of the wet material of ditrihydroxy is significantly reduced, and the content is above 98%.

[0044] The specific implementation methods described above further illustrate the objectives, technical solutions and beneficial effects of the present invention in detail. It should be understood that the above description is only a specific implementation method of the present invention and is not intended to limit the scope of protection of the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A method for removing colored impurities from a ditrihydroxy material, characterized in that: The colored impurity removal method comprises: S100, putting the heavy component and the solvent into a preparation tank, stirring, adding the mother liquor and deionized water for preparation, stirring evenly and heating to 80-85° C., and standing for 30 minutes to obtain a mixed material; S200, sending the mixed material into a separator to separate the water phase and the oil phase, and washing the oil phase with water to obtain an extracted water phase product; S300, heating and concentrating the aqueous phase product after extraction to concentrate 40% of the water in the aqueous phase product; S400, the concentrated aqueous phase product enters the activated carbon preparation tank for decolorization, is stirred at 60°C for 30 minutes and phosphoric acid is added for hydrolysis, and the pH value is adjusted to 3.0-3.5; S500, filtering the concentrated solution after hydrolysis and decolorization, cooling and crystallizing, and preparing a bistrihydroxy material.

2. The method for removing colored impurities in a bistrihydroxy material according to claim 1, characterized in that: The mass ratio of the heavy component to the solvent in step S100 is 1:1, and the mixture is stirred for 15 minutes before adding the mother liquor and deionized water. The addition ratio of the mother liquor is 5 times that of the heavy component, and the addition ratio of deionized water is 2 times that of the heavy component.

3. The method for removing colored impurities in a bistrihydroxy material according to claim 1, characterized in that: The solvent in step S100 is isooctyl alcohol.

4. The method for removing colored impurities in a bistrihydroxy material according to claim 1, characterized in that: The separator in step S200 is a separation tower, and the mixed material enters the separation tower from the middle, and the water washing temperature is 90°C.

5. The method for removing colored impurities in a bistrihydroxy material according to claim 1, characterized in that: The temperature of the heating and concentration in step S300 is 98-102°C.

6. The method for removing colored impurities in a bistrihydroxy material according to claim 1, characterized in that: The amount of activated carbon added to the activated carbon preparation tank in step S400 is 0.3% of the total mass of the concentrated aqueous phase product.

7. The method for removing colored impurities in a bistrihydroxy material according to claim 1, characterized in that: The amount of phosphoric acid added in step S400 is 0.3-0.5% of the total mass of the concentrated aqueous phase product, and the hydrolysis time is 1 hour.

8. A ditrihydroxy material, characterized in that The bistrihydroxy material is prepared according to the method for removing colored impurities from the bistrihydroxy material according to any one of claims 1 to 7, The wet material chromaticity of the ditrihydroxy material crystal is less than 30, ditrimethylolpropane is ≥98%, and impurities are less than 2%.

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