CN105273206A - Globular alkali lignin amine-mixing type anion exchanger and preparation method thereof - Google Patents
Globular alkali lignin amine-mixing type anion exchanger and preparation method thereof Download PDFInfo
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- CN105273206A CN105273206A CN201510827506.4A CN201510827506A CN105273206A CN 105273206 A CN105273206 A CN 105273206A CN 201510827506 A CN201510827506 A CN 201510827506A CN 105273206 A CN105273206 A CN 105273206A
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Abstract
The invention relates to a globular alkali lignin amine-mixing type anion exchanger and a preparation method thereof and belongs to the technical field of high polymer materials. The globular alkali lignin amine-mixing type anion exchanger provided by the invention comprises the following raw materials in parts by weight: 30-50 parts of alkali lignin white ball, 200-300 parts of epoxy chloropropane, 40-60 parts of acetic ether, 10-20 parts of perchloric acid, 40-60 parts of deionized water, 500-700 parts of ethyl alcohol, 500-600 parts of acetone, 300-400 parts of 1N HCI, 300-400 parts of 1N NaOH, 100-150 parts of diethylamine and 100-150 parts of quadrol. The invention provides a new technical method for preparing the globular alkali lignin amine-mixing type anion exchanger, the product quality is high and the yield is high.
Description
Technical field
The present invention relates to a kind of anionite and preparation method thereof, more particularly, the present invention relates to a kind of spherical alkali lignin and mix amine type anionite and preparation method thereof, belong to technical field of polymer materials.
Background technology
Natural art element is the high molecular polymer that phenylpropane units is formed, and complex structure, exists several functions base in molecule, as methoxyl group (-OCH), hydroxyl (-OH) and carbonyl (-CO-) etc.During lignin balling-up, to be cross-linked with each other formation by its hydroxyl.And alkali art element is plant material or paper pulp boiling together with alkali, by a kind of brown precipitate thing obtained after alkali lye acidifying, so the more general lignin of this element of alkali has new free phenolic hydroxyl group, after being cross-linked to form Archon, remaining hydroxyl is had not participate in reaction.
Existing spherical alkali lignin mixes amine type anionite and has remaining hydroxyl and do not participate in reaction, and obtained spherical alkali lignin to mix amine type anionite of low quality, yield is low.
Summary of the invention
The present invention is intended to solve spherical alkali lignin in prior art and mixes the problem of amine type anionite, and provide a kind of spherical alkali lignin to mix amine type anionite, whole hydroxyl can be made to participate in reaction, and the quality product obtained is high, and yield is high.
In order to realize foregoing invention object, its concrete technical scheme is as follows:
A kind of spherical alkali lignin mixes amine type anionite, it is characterized in that: comprise the following raw material according to weight parts:
Alkali lignin Archon 30-50 part
Epoxy chloropropane 200-300 part
Vinyl acetic monomer 40-60 part
Perchloric acid 10-20 part
Deionized water 40-60 part
Alcohol 500-700 part
Acetone 500-600 part
1NHCI300-400 part
1NNaOH300-400 part
Diethylamine 100-150 part
Quadrol 100-150 part.
Spherical alkali lignin mixes a preparation method for amine type anionite, it is characterized in that: comprise following processing step:
A, in there-necked flask, add acetone and be warming up to 50-55 DEG C, then adding alkali lignin Archon, swelling 0.5-1.0h under slow stirring; Add epoxy chloropropane, fully stir, control temperature of reaction at 50-55 DEG C, drip high chloro acid solution; Dropwise rear continuation reaction 2-3h;
B, suction filtration go out reaction product, use alcohol repetitive scrubbing, namely obtain epoxidation alkali lignin Archon intermediate after drying;
C, in another reactor, add the epoxidation alkali lignin Archon intermediate of step B, add alcohol and swelling treatment 1-2h is continued to epoxidation alkali lignin Archon; Temperature of reaction system is risen to 60-65 DEG C;
D, add diethylamine and quadrol, maintain temperature of reaction 60-65 DEG C of reaction 2-3h; Be warming up to 65-70 DEG C, continue reaction 2-3h; Cooling, leaches reaction product; Ethanol wash, dry that spherical alkali lignin mixes amine type anionite.
In step, described dropping high chloro acid solution refers to and to dropwise in 3-4h in the present invention.
In stepb, described is washing 3-5 time with alcohol repetitive scrubbing in the present invention.
In stepb, the temperature of described drying is 60-80 DEG C in the present invention.
The Advantageous Effects that the present invention brings:
The invention solves spherical alkali lignin in prior art to mix amine type anionite and have remaining hydroxyl not participate in reaction, and obtained spherical alkali lignin to mix amine type anionite of low quality, the problem that yield is low.The present invention adopts indirect etherification method, first by spherical alkali lignin Archon and epoxy chloropropane under the catalysis of acid, synthesize 3-chlorine-2-hydroxyl propyl group alkali lignin ether, and then and diethylamine, reacting ethylenediamine, namely obtained spherical alkali lignin diethylamine, diamine type mix amine anionite, mix amine type anionite provide a technical strategies for preparing alkali lignin, quality product is high, and yield is high.
Embodiment
embodiment 1
A kind of spherical alkali lignin mixes amine type anionite, comprises the following raw material according to weight parts:
Alkali lignin Archon 30 parts
Epoxy chloropropane 200 parts
Vinyl acetic monomer 40 parts
10 parts, perchloric acid
Deionized water 40 parts
Alcohol 500 parts
500 parts, acetone
1NHCI300 part
1NNaOH300 part
Diethylamine 100 parts
Quadrol 100 parts.
embodiment 2
A kind of spherical alkali lignin mixes amine type anionite, comprises the following raw material according to weight parts:
Alkali lignin Archon 50 parts
Epoxy chloropropane 300 parts
Vinyl acetic monomer 60 parts
20 parts, perchloric acid
Deionized water 60 parts
Alcohol 700 parts
600 parts, acetone
1NHCI400 part
1NNaOH400 part
Diethylamine 150 parts
Quadrol 150 parts.
embodiment 3
A kind of spherical alkali lignin mixes amine type anionite, comprises the following raw material according to weight parts:
Alkali lignin Archon 40 parts
Epoxy chloropropane 250 parts
Vinyl acetic monomer 450 parts
15 parts, perchloric acid
Deionized water 50 parts
Alcohol 600 parts
550 parts, acetone
1NHCI350 part
1NNaOH350 part
Diethylamine 125 parts
Quadrol 125 parts.
embodiment 4
A kind of spherical alkali lignin mixes amine type anionite, comprises the following raw material according to weight parts:
Alkali lignin Archon 33 parts
Epoxy chloropropane 220 parts
Vinyl acetic monomer 57 parts
11 parts, perchloric acid
Deionized water 46 parts
Alcohol 560 parts
570 parts, acetone
1NHCI330 part
1NNaOH380 part
Diethylamine 105 parts
Quadrol 135 parts.
embodiment 5
Spherical alkali lignin mixes a preparation method for amine type anionite, comprises following processing step:
A, in there-necked flask, add acetone and be warming up to 50 DEG C, then adding alkali lignin Archon, swelling 0.5h under slow stirring; Add epoxy chloropropane, fully stir, control temperature of reaction at 50 DEG C, drip high chloro acid solution; Dropwise rear continuation reaction 2h;
B, suction filtration go out reaction product, use alcohol repetitive scrubbing, namely obtain epoxidation alkali lignin Archon intermediate after drying;
C, in another reactor, add the epoxidation alkali lignin Archon intermediate of step B, add alcohol and swelling treatment 1h is continued to epoxidation alkali lignin Archon; Temperature of reaction system is risen to 60 DEG C;
D, add diethylamine and quadrol, maintain temperature of reaction 60 DEG C reaction 2h; Be warming up to 65 DEG C, continue reaction 2h; Cooling, leaches reaction product; Ethanol wash, dry that spherical alkali lignin mixes amine type anionite.
Preferred:
In step, described dropping high chloro acid solution refers to and to dropwise in 3h.
In stepb, described is washing 3 times with alcohol repetitive scrubbing.
In stepb, the temperature of described drying is 60 DEG C.
embodiment 6
Spherical alkali lignin mixes a preparation method for amine type anionite, comprises following processing step:
A, in there-necked flask, add acetone and be warming up to 55 DEG C, then adding alkali lignin Archon, swelling 1.0h under slow stirring; Add epoxy chloropropane, fully stir, control temperature of reaction at 55 DEG C, drip high chloro acid solution; Dropwise rear continuation reaction 3h;
B, suction filtration go out reaction product, use alcohol repetitive scrubbing, namely obtain epoxidation alkali lignin Archon intermediate after drying;
C, in another reactor, add the epoxidation alkali lignin Archon intermediate of step B, add alcohol and swelling treatment 2h is continued to epoxidation alkali lignin Archon; Temperature of reaction system is risen to 65 DEG C;
D, add diethylamine and quadrol, maintain temperature of reaction 65 DEG C reaction 3h; Be warming up to 70 DEG C, continue reaction 3h; Cooling, leaches reaction product; Ethanol wash, dry that spherical alkali lignin mixes amine type anionite.
Preferred:
In step, described dropping high chloro acid solution refers to and to dropwise in 4h.
In stepb, described is washing 5 times with alcohol repetitive scrubbing.
In stepb, the temperature of described drying is 80 DEG C.
embodiment 7
Spherical alkali lignin mixes a preparation method for amine type anionite, comprises following processing step:
A, in there-necked flask, add acetone and be warming up to 52.5 DEG C, then adding alkali lignin Archon, swelling 0.75h under slow stirring; Add epoxy chloropropane, fully stir, control temperature of reaction at 52.5 DEG C, drip high chloro acid solution; Dropwise rear continuation reaction 2.5h;
B, suction filtration go out reaction product, use alcohol repetitive scrubbing, namely obtain epoxidation alkali lignin Archon intermediate after drying;
C, in another reactor, add the epoxidation alkali lignin Archon intermediate of step B, add alcohol and swelling treatment 1.5h is continued to epoxidation alkali lignin Archon; Temperature of reaction system is risen to 62.5 DEG C;
D, add diethylamine and quadrol, maintain temperature of reaction 62.5 DEG C reaction 2.5h; Be warming up to 67.5 DEG C, continue reaction 2.5h; Cooling, leaches reaction product; Ethanol wash, dry that spherical alkali lignin mixes amine type anionite.
Preferred:
In step, described dropping high chloro acid solution refers to and to dropwise in 3.5h.
In stepb, described is washing 4 times with alcohol repetitive scrubbing.
In stepb, the temperature of described drying is 70 DEG C.
embodiment 8
Spherical alkali lignin mixes a preparation method for amine type anionite, comprises following processing step:
A, in there-necked flask, add acetone and be warming up to 51 DEG C, then adding alkali lignin Archon, swelling 0.9h under slow stirring; Add epoxy chloropropane, fully stir, control temperature of reaction at 52 DEG C, drip high chloro acid solution; Dropwise rear continuation reaction 2.25h;
B, suction filtration go out reaction product, use alcohol repetitive scrubbing, namely obtain epoxidation alkali lignin Archon intermediate after drying;
C, in another reactor, add the epoxidation alkali lignin Archon intermediate of step B, add alcohol and swelling treatment 1.75h is continued to epoxidation alkali lignin Archon; Temperature of reaction system is risen to 64.5 DEG C;
D, add diethylamine and quadrol, maintain temperature of reaction 62 DEG C reaction 2.75h; Be warming up to 69 DEG C, continue reaction 2.25h; Cooling, leaches reaction product; Ethanol wash, dry that spherical alkali lignin mixes amine type anionite.
Preferred:
In step, described dropping high chloro acid solution refers to and to dropwise in .25h.
In stepb, described is washing 4 times with alcohol repetitive scrubbing.
In stepb, the temperature of described drying is 72 DEG C.
Claims (5)
1. spherical alkali lignin mixes an amine type anionite, it is characterized in that: comprise the following raw material according to weight parts:
Alkali lignin Archon 30-50 part
Epoxy chloropropane 200-300 part
Vinyl acetic monomer 40-60 part
Perchloric acid 10-20 part
Deionized water 40-60 part
Alcohol 500-700 part
Acetone 500-600 part
1NHCI300-400 part
1NNaOH300-400 part
Diethylamine 100-150 part
Quadrol 100-150 part.
2. a kind of spherical alkali lignin according to claim 1 mixes the preparation method of amine type anionite, it is characterized in that: comprise following processing step:
A, in there-necked flask, add acetone and be warming up to 50-55 DEG C, then adding alkali lignin Archon, swelling 0.5-1.0h under slow stirring; Add epoxy chloropropane, fully stir, control temperature of reaction at 50-55 DEG C, drip high chloro acid solution; Dropwise rear continuation reaction 2-3h;
B, suction filtration go out reaction product, use alcohol repetitive scrubbing, namely obtain epoxidation alkali lignin Archon intermediate after drying;
C, in another reactor, add the epoxidation alkali lignin Archon intermediate of step B, add alcohol and swelling treatment 1-2h is continued to epoxidation alkali lignin Archon; Temperature of reaction system is risen to 60-65 DEG C;
D, add diethylamine and quadrol, maintain temperature of reaction 60-65 DEG C of reaction 2-3h; Be warming up to 65-70 DEG C, continue reaction 2-3h; Cooling, leaches reaction product; Ethanol wash, dry that spherical alkali lignin mixes amine type anionite.
3. a kind of spherical alkali lignin according to claim 2 mixes the preparation method of amine type anionite, it is characterized in that: in step, and described dropping high chloro acid solution refers to and to dropwise in 3-4h.
4. a kind of spherical alkali lignin according to claim 2 mixes the preparation method of amine type anionite, it is characterized in that: in stepb, and described is washing 3-5 time with alcohol repetitive scrubbing.
5. a kind of spherical alkali lignin according to claim 2 or 4 mixes the preparation method of amine type anionite, it is characterized in that: in stepb, and the temperature of described drying is 60-80 DEG C.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85100892A (en) * | 1985-04-01 | 1986-01-10 | 中国科学院化学研究所 | Papery amberplex and method for making thereof and be applied to the electrodialysis clean water treatment |
| CN1597118A (en) * | 2004-07-28 | 2005-03-23 | 南京工业大学 | Quaternary ammonium type anion exchange agent and its preparation method |
| CN101698157A (en) * | 2009-10-23 | 2010-04-28 | 山东大学 | Anion-exchange agent prepared by using fermented straws, preparation method thereof and use thereof |
| CN104411712A (en) * | 2012-05-03 | 2015-03-11 | 威尔迪亚有限公司 | Methods for treating lignocellulosic materials |
| CN104826671A (en) * | 2015-04-30 | 2015-08-12 | 王英英 | Preparation method for hydroxyethyldimethylamino group monodispersive highly-basic anion exchanger |
-
2015
- 2015-11-25 CN CN201510827506.4A patent/CN105273206A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85100892A (en) * | 1985-04-01 | 1986-01-10 | 中国科学院化学研究所 | Papery amberplex and method for making thereof and be applied to the electrodialysis clean water treatment |
| CN1597118A (en) * | 2004-07-28 | 2005-03-23 | 南京工业大学 | Quaternary ammonium type anion exchange agent and its preparation method |
| CN101698157A (en) * | 2009-10-23 | 2010-04-28 | 山东大学 | Anion-exchange agent prepared by using fermented straws, preparation method thereof and use thereof |
| CN104411712A (en) * | 2012-05-03 | 2015-03-11 | 威尔迪亚有限公司 | Methods for treating lignocellulosic materials |
| CN104826671A (en) * | 2015-04-30 | 2015-08-12 | 王英英 | Preparation method for hydroxyethyldimethylamino group monodispersive highly-basic anion exchanger |
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Application publication date: 20160127 |