Method for synthesizing diethanol amide

CN102702009A
China
Abstract
The invention discloses a method for synthesizing diethanol amide and belongs to
the technical field of synthesis of amides compounds in organic chemistry.
According to the method, fatty acid methyl ester and diethanol amine which are
used as raw materials are subjected to amidation under the action of catalyst to
form diethanol amide, wherein the molar ratio of fatty acid methyl ester to
diethanol amine is 1:(1.0-1.1), the catalyst is sodium methoxide or potassium
hydroxide, and the adding amount of the catalyst is 0.5 to 1.0 percent based on the
total mass of fatty acid methyl ester and diethanol amine. According to the method,
diethanol amide of which the molar ratio of fatty acid methyl ester to diethanol
amine is 1:1 can be synthesized by a one-step method; and the process is simple,
and materials are low in cost.
Description
A kind of compound method of fatty diglycollic amide
Technical field
The present invention has set forth a kind of compound method of fatty diglycollic
amide, belongs to the synthesis technical field of the amides in the organic
chemistry.
Background technology
The fatty diglycollic amide general formula is RCON (CH 2-CH 2OH) 2, weak
yellow liquid, nontoxic, nonirritant, solubleness reduces, increases with the
temperature rising with the increase of carbonatoms.Change methyl esters and
diethylolamine amount of substance ratio, can prepare water-soluble better
alkylolamide.
Alkylol amide has the surface of good activity; It is one of most important kind in
the nonionogenic tenside; Be actives monomer important in the modern synthetic
detergent, be widely used in washing composition, suds-stabilizing agent,
thickening material, softening agent, rust-preventive agent, static inhibitor etc.And
the effect aspect TOR is also very good, can reach the ultra low interfacial tension
of 1OmN/m, but also fewer in the application in field, oil field, now has much
human to carry out the research of this respect both at home and abroad.
Summary of the invention
In view of the above problems, the present invention has adopted a kind of
technology simple and easy, easy to operate, with low cost and can effectively
prepare the compound method of highly purified fatty diglycollic amide.Concrete
scheme is following:
A kind of compound method of fatty diglycollic amide is a raw material with fatty
acid methyl ester and diethylolamine, under the effect of basic catalyst, carries out
amidate action and obtains said fatty diglycollic amide;
The mol ratio of said fatty acid methyl ester and said diglycollic amide is 1:1.0～
1.1;
Said basic catalyst is sodium methylate or sodium hydroxide, and its add-on is 0.5
～1.0% of fatty acid methyl ester and a diethylolamine gross weight;
The temperature of said amidate action is 100～120 ℃, and vacuum tightness is
0.03～0.05MPa, and the reaction times is 2～4 hours.
Said fatty acid methyl ester is coconut oil fatty acid methyl ester, palm-kernel oil
fatty acid methyl ester or palm oil fatty acid methyl esters.
The by product of said amidate action is thick methyl alcohol, after the subsequent
handling purification, can be used for producing fatty acid methyl ester.
The present invention compared with prior art has following outstanding advantage
and positively effect.
1, adopt the synthetic 1:1 type fatty diglycollic amide of single stage method,
technology is simple;
2, reaction conditions is gentle, and the equipment of employing is simple, and
Material Cost is cheap.
By the fatty diglycollic amide of synthetic fatty acid methyl ester of the present
invention and diethylolamine 1:1 type, purity can be widely used in washing
composition, suds-stabilizing agent, thickening material, softening agent, rust-
preventive agent, static inhibitor etc. greater than 90%.
Embodiment
Below, further specify content of the present invention with embodiment, but
protection scope of the present invention is not limited in embodiment.The
variation and the modification of other that those skilled in the art is made under
the situation that does not deviate from the present invention spirit and protection
domain still are included within the protection domain of the present invention.
Embodiment 1
In reaction kettle, add 720 parts of coconut oil fatty acid methyl esters and 330
parts of diethanolamine in proportion, under agitation add 8.5 parts of sodium
methylates, closed reactor changes and slow is warming up to 115 ℃, and vacuum
tightness is 0.05MPa, and the reaction times is 4 hours.The methyl alcohol that
distills out after the subsequent handling purification, can be used for producing
fatty acid methyl ester.Resources conservation and refuse zero release.Amide
content is greater than 92% in the cocoanut fatty acid diethanolamide that building-
up reactions obtains, and unhindered amina content is less than 5%, and free fatty
acid content is less than 1%.
Embodiment 2
In reaction kettle, add 705 palm-kernel oil fatty acid methyl esters and 330 parts of
diethanolamine in proportion, under agitation add 9.5 parts of sodium methylates,
closed reactor changes and slow is warming up to 120 ℃, and vacuum tightness is
0.03MPa, and the reaction times is 2 hours.The methyl alcohol that distills out after
the subsequent handling purification, can be used for producing fatty acid methyl
ester.Resources conservation and refuse zero release.Amide content is greater than
94% in the palm-kernel oil fatty diglycollic amide that building-up reactions
obtains, and unhindered amina content is less than 5%, and free fatty acid content
is less than 1%.
Embodiment 3
In reaction kettle, add 705 palm oil fatty acid methyl esters and 320 parts of
diethanolamine in proportion, under agitation add 9.2 parts of sodium methylates,
closed reactor changes and slow is warming up to 100 ℃, and vacuum tightness is
0.04MPa, and the reaction times is 3 hours.The methyl alcohol that distills out after
the subsequent handling purification, can be used for producing fatty acid methyl
ester.Resources conservation and refuse zero release.Amide content is greater than
93% in the palm-kernel oil fatty diglycollic amide that building-up reactions
obtains, and unhindered amina content is less than 5%, and free fatty acid content
is less than 1%.
Claims (3)
1. the compound method of a fatty diglycollic amide is characterized in that, is raw
material with fatty acid methyl ester and diethylolamine, under the effect of basic
catalyst, carries out amidate action and obtains said fatty diglycollic amide;
The mol ratio of said fatty acid methyl ester and said diglycollic amide is 1:1.0～
1.1;
Said basic catalyst is sodium methylate or sodium hydroxide, and its add-on is 0.5
～1.0% of said fatty acid methyl ester and a diethylolamine gross weight;
The temperature of said amidate action is 100～120 ℃, and vacuum tightness is
0.03～0.05MPa, and the reaction times is 2～4 hours.
2. compound method according to claim 1 is characterized in that, said fatty acid
methyl ester is coconut oil fatty acid methyl ester, palm-kernel oil fatty acid methyl
ester or palm oil fatty acid methyl esters.
3. compound method according to claim 1 is characterized in that, the by product
of said amidate action is thick methyl alcohol, after the subsequent handling
purification, can be used for producing fatty acid methyl ester.