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A kind of lignin cyclic amine cationic asphalt emulsifier and preparation method thereof

An asphalt emulsifier, cationic technology, applied in building components, building insulation materials, buildings, etc., can solve the problems of high requirements for production and experimental equipment, high cost of emulsifier raw materials, cumbersome preparation steps, etc., to achieve low production costs and increase Emulsifying performance, the effect of simple process

Inactive Publication Date: 2018-06-12
SHANDONG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage of this method is that the preparation steps are cumbersome, the cost is high, and high temperature reaction is required
[0005] The general disadvantages of the above cationic asphalt emulsifiers and their preparation methods are: the cost of raw materials for the preparation of emulsifiers is high, the sources are limited, high temperature reactions are required during preparation, and the requirements for production and experimental equipment are relatively high

Method used

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  • A kind of lignin cyclic amine cationic asphalt emulsifier and preparation method thereof
  • A kind of lignin cyclic amine cationic asphalt emulsifier and preparation method thereof
  • A kind of lignin cyclic amine cationic asphalt emulsifier and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0049] (1) Preparation of lignin cyclic amine cationic asphalt emulsifier:

[0050] 1) Add 129.0 g of N-aminoethylpiperazine into the reactor, then dropwise add 72.1 g of acrylic acid, and stir at 45° C. for 1 h to obtain reaction intermediate I.

[0051] 2) In another reactor, add 193.1g of 33% (mass fraction) trimethylamine aqueous solution, gradually add 131.2g of 30% (mass fraction) industrial hydrochloric acid, then gradually add 97.1g of epichlorohydrin, and stir and react at 45°C for 2h to obtain Reaction Intermediate II.

[0052] 3) In another reactor, 283.0 g of lignin was dissolved in 649.6 g of 10.7% (mass fraction) sodium hydroxide aqueous solution, mixed and stirred for reaction to obtain reaction intermediate III.

[0053] 4) Add reaction intermediate I to reaction intermediate III, then gradually add 92.5 g of 37% (mass fraction) formaldehyde, and react at 70°C for 3 hours to obtain reaction intermediate IV;

[0054] 5) Gradually add the reaction intermediate ...

Embodiment 2

[0064] (1) Preparation of lignin cyclic amine cationic asphalt emulsifier:

[0065] 1) Add 129.0 g of N-aminoethylpiperazine into the reactor, then dropwise add 72.1 g of acrylic acid, and stir at 45° C. for 1 h to obtain reaction intermediate I.

[0066] 2) Add 109.1g triethylamine to another reactor, gradually add 131.2g 30% (mass fraction) industrial hydrochloric acid, then gradually add 97.1g epichlorohydrin, stir and react at 45°C for 2h to obtain reaction intermediate II.

[0067] 3) In another reactor, 283.0 g of lignin was dissolved in 649.6 g of 10.7% (mass fraction) sodium hydroxide aqueous solution, mixed and stirred for reaction to obtain reaction intermediate III.

[0068] 4) Add reaction intermediate I to reaction intermediate III, then gradually add 92.5 g of 37% (mass fraction) formaldehyde, and react at 60°C for 4 hours to obtain reaction intermediate IV;

[0069] 5) Gradually add the reaction intermediate II to the reaction intermediate IV, and react at 80° ...

Embodiment 3

[0078] (1) Preparation of lignin cyclic amine cationic asphalt emulsifier:

[0079] 1) Add 129.0 g of N-aminoethylpiperazine into the reactor, then dropwise add 72.1 g of acrylic acid, and stir at 45° C. for 1 h to obtain reaction intermediate I.

[0080] 2) In another reactor, add 189.6g 85% (mass fraction) triethanolamine aqueous solution, gradually add 131.2g 30% (mass fraction) industrial hydrochloric acid, then gradually add 97.1g epichlorohydrin, stir and react at 45°C for 2h, Reaction intermediate II is obtained.

[0081] 3) In another reactor, 283.0 g of lignin was dissolved in 649.6 g of 10.7% (mass fraction) sodium hydroxide aqueous solution, mixed and stirred for reaction to obtain reaction intermediate III.

[0082] 4) Add the reaction intermediate I to the reaction intermediate III, then gradually add 92.5g of 37% (mass fraction) formaldehyde, react at 80°C for 2 hours, and obtain the reaction intermediate IV;

[0083] 5) Gradually add the reaction intermediate ...

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Abstract

The invention discloses a lignin cyclamine cationic-type asphalt emulsifier and a preparation method and application thereof. The molecular structure general formula of the emulsifier is as shown in the description, wherein R is a methyl group (-CH3) or an ethyl group (-C2H5) or a hydroxyethyl group (-C2H4OH), and LIGNIN represents a lignin molecular chain. The lignin cyclamine cationic-type asphalt emulsifier is prepared from, by mass, 100 parts of lignin, 159-230 parts of water, 19-27 parts of sodium hydroxide, 42-50 parts of N-aminoethylpiperazine, 23-29 parts of acrylic acid, 30-36 parts of formaldehyde (37%), 35-82 parts of tertiary amine with a low carbon number, 42-50 parts of industrial hydrochloric acid (30%) and 31-37 parts of epoxy chloropropane. According to the lignin cyclamine cationic-type asphalt emulsifier, the synthesis raw materials are easy to obtain, the production cost is low, the technology is simple, and high-temperature reacting is not needed; the emulsifier can emulsify different types of asphalt, the prepared emulsified asphalt is fine and uniform, the storage stability is good, and rapid-cracking cationic-type emulsified asphalt can be prepared.

Description

technical field [0001] The invention relates to a lignin cyclic amine cationic asphalt emulsifier and a preparation method thereof, belonging to the technical field of fine chemicals. Background technique [0002] Emulsified asphalt is an oil-in-water liquid asphalt emulsion formed by asphalt and water under the action of an emulsifier. Emulsified asphalt is mainly divided into cationic emulsified asphalt, anionic emulsified asphalt and nonionic emulsified asphalt. Among them, cationic emulsified asphalt is widely used in road construction and road maintenance due to its energy-saving and environmental protection, can improve construction conditions, has strong adhesion to stone materials, and can effectively reduce over-aging of asphalt and many other excellent application characteristics. [0003] The most critical factor affecting the road performance of emulsified asphalt is the asphalt emulsifier. At present, the main varieties of cationic asphalt emulsifiers at home a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08H7/00C08J3/03C08L95/00
CPCC08H6/00C08J3/03C08J2395/00C08L95/00
Inventor 施来顺王天曜李德梅陈孟马存飞
Owner SHANDONG UNIV
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