Hydroxymethylated lignin and application thereof

A technology of hydroxymethylation and lignin, which is applied in the application of said hydroxymethylation lignin, hydroxymethylation lignin, and the application field in the preparation of polyurethane foam, to reduce costs, reduce particle size, highly active effect

Active Publication Date: 2013-07-31
JINAN SHENGQUAN GRP SHARE HLDG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problem that the above lignin hydroxyl content is low, resulting in its low activity and limiting its application in the preparation of polyurethane foam, the present invention provides a Hydroxymethylated lignin with high hydroxyl content and high activity

Method used

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  • Hydroxymethylated lignin and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Take corn cob lignin black liquor with 100 parts of absolute dry lignin, add it to the reaction bottle, add 10 parts, 25 parts, 40 parts, 55 parts, and 70 parts of formaldehyde solution respectively, and react at 70 °C for 1 hour. Add 3 parts, 6 parts, 9 parts, 12 parts, and 15 parts of acetone, respectively numbered ①, ②, ③, ④, ⑤, continue the reaction for 1 hour, cool to room temperature, acidify, filter, and dry to obtain hydroxymethyl lignin. The hydroxyl value data of the obtained hydroxymethyl lignin are shown in Table 1.

[0039] Table 1

[0040]

[0041] Known by above-mentioned data, when taking absolute dry lignin as 100 parts of corn cob lignin black liquor, when formaldehyde solution add-on is 70 parts, the hydroxyl value of gained hydroxymethylated lignin in the value range of formaldehyde solution is maximum, Due to the consideration of the cost of raw materials, the amount of 70 parts of formaldehyde solution is used as an appropriate amount.

Embodiment 2

[0043] Take corncob lignin black liquor with 100 parts of absolute dry lignin, add it to the reaction bottle, add 70 parts of formaldehyde solution, and react for 1 hour at 70°C, add 4 parts, 8 parts, 12 parts, and 15 parts of Acetone, respectively numbered ⑥, ⑦, ⑧, ⑨, continued to react for 1 hour, cooled to room temperature, acidified, filtered, and dried to obtain hydroxymethylated lignin. In the process of filtering, see Table 2 for the influence of the amount of acetone added on the filtration rate.

[0044] Table 2

[0045] Numbering Amount of formaldehyde solution / part Addition amount of acetone / part Filtration rate / (mL / min) ⑥ 70 4 102 ⑦ 70 8 120 ⑧ 70 12 150 ⑨ 70 15 152

[0046] It can be seen from the above data that the dispersion uniformity is improved after adding acetone. When the amount of acetone added is 12 parts, the filtration rate of the modified lignin is significantly improved, and after continuing to add ace...

Embodiment 3

[0049] Take 10 parts of hydroxymethylated lignin numbered ⑧ in Example 2, dry it in vacuum at 50°C for 2 hours, add 100 parts of polyethylene glycol 400, 1.5 parts of triethylenediamine, 0.1 part of dibutyldiamine Lauric acid, 0.5 parts of water, 25 parts of cyclopentane, 2.5 parts of silicone oil, mix evenly under stirring, quickly add 110 parts of PM 200, stir and mix evenly, pour into a mold preheated to 40-50°C, and carry out After foaming, take out the foam body and cure at room temperature to obtain a hydroxymethylated lignin modified polyurethane rigid foam with a thermal conductivity of 0.0193 w / m k (25°C) and a closed cell rate of 93.7%. The intensity is 230.98Kpa.

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Abstract

The invention relates to the technical field of organic chemical engineering, especially a hydroxymethylated lignin which is prepared by the following steps: after filtering lignin with black liquor, reacting with formaldehyde at 60-90 DEG C for 1-2 hours, adding acetone to continue the reaction for 1-2 hours, cooling to room temperature after the reaction finishes, carrying out acid precipitation, filtering and drying to obtain the hydroxymethylated lignin. The invention also relates to application of the hydroxymethylated lignin in preparing polyurethane foam. The used lignin is corn cob lignin black liquor, the production conditions are mild, and the lignin in the black liquor still has the structure of the natural lignin and has higher hydroxy content and higher compatibility with polyether glycol; and thus, the hydroxymethylated lignin has the advantages of higher activity, higher purity and higher dispersity. When being used for preparing polyurethane hard foam, the hydroxymethylated lignin lowers the production cost, has excellent properties and enhances the competitive power of the product.

Description

technical field [0001] The invention relates to the technical field of organic chemical industry, in particular to a hydroxymethylated lignin, and also relates to the application of the hydroxymethylated lignin. Background technique [0002] Lignin is an inexhaustible natural renewable resource, which together with cellulose and hemicellulose constitutes the basic skeleton of plants. In the production process, it is often discharged into the environment as waste, causing waste of resources and environmental pollution. [0003] Polyurethane rigid foam is widely used in refrigerators, freezers and construction fields as a good thermal insulation material due to its low thermal conductivity, good thermal insulation, light weight, and chemical corrosion resistance. However, due to the increasing depletion of petroleum resources and the rising price of raw materials, the production cost and selling price of rigid polyurethane foam are relatively high, which seriously affects i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08H7/00C08G18/64
Inventor 唐一林江成真张丽伟焦峰
Owner JINAN SHENGQUAN GRP SHARE HLDG CO LTD
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