CN108249792A - A kind of preparation method of polypeptide calcium sulphate retarder - Google Patents
A kind of preparation method of polypeptide calcium sulphate retarder Download PDFInfo
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- CN108249792A CN108249792A CN201810069496.6A CN201810069496A CN108249792A CN 108249792 A CN108249792 A CN 108249792A CN 201810069496 A CN201810069496 A CN 201810069496A CN 108249792 A CN108249792 A CN 108249792A
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- polypeptide
- retarder
- preparation
- calcium sulphate
- gypsum
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B11/00—Calcium sulfate cements
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/28—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/30—Condensation polymers of aldehydes or ketones
- C04B24/305—Melamine-formaldehyde condensation polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
- C08G12/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08G12/30—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with substituted triazines
- C08G12/32—Melamines
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/20—Retarders
- C04B2103/22—Set retarders
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Phenolic Resins Or Amino Resins (AREA)
Abstract
The invention discloses a kind of preparation method of polypeptide calcium sulphate retarder, based on polypeptide is hydrophilic and close calcium feature, chemical modification has been carried out to albumen.Using polypeptide after collagen degradation a kind of dendrimer is synthesized with nitrogenous polyhydroxy methyl.The retarder has good dispersion water retaining function, does not crystallize in gypsum and does not assemble, does not influence gypsum crystal and formed, and it is more than 300min to obtain Slow setting time, keeps gypsum intensity preferable.Reach national 3 grades of standards of building gypsum (GB/T 9,776 2008) after sample detection.
Description
Technical field
The present invention relates to calcium sulphate retarder technical field more particularly to the resins of a kind of polypeptide and melamine condensation
Prepare calcium sulphate retarder.
Background technology
Retarder is one of necessary components of all kinds of gypsum base materials such as brushing gypsum, gypsum base putty, model plaster.Mesh
Preceding common retarder mainly has three classes：Inorganic phosphate, organic multi-carboxylate and protein-based.Organic acid retarder
Mainly there are citric acid, tartaric acid, acrylic acid etc., inorganic phosphate salt retarder mainly has calgon, sodium polyphosphate etc.,
Protein-based retarder includes gelatine, collagen polypeptide etc..Calcium sulphate retarder all can inevitably give gypsum while slow setting
The intensity of hardenite is brought a negative impact.In general, Slow setting time is longer, and strength reduction amplitude is bigger.Such as common albumen
Retarder makes the gypsum presetting period when extending to 6h, and loss of strength is more than 30%；Using organic acid retarder, make gypsum
When presetting period extends to 4h, loss of strength is more than 50%；.Therefore, influence one of the retarder to gypsum intensity how is reduced
It is directly the important topic of retarder research.
Protein-based retarder is smaller to the damage of gypsum intensity.It develops novel protein-based retarder and is also caused pass
Note.The deferred action of protein-based retarder derives from the water retention of protein colloid itself, to the crystal of dihydrate gypsum
Ultimately form and change influence it is smaller, it is thus smaller to its loss of strength.Protein-based big in molecular weight, intermolecular combination is strong,
Contraction is formed into intramolecular or intermolecular combination in the environment of different boundary's electric constants, reduces the binding site of water.Straight chain albumen
Polypeptide can be dispersed in gypsum body, but for slow setting, and a large amount of polypeptide intervention will reduce the crystallizing power of gypsum or change
Metacrystal volume morphing.Stablize to reduce the contact promise crystal volume between gypsum crystal.The albumen of bigger molecule alkali,
Heat and oxidant (including air) effect decline solution occur two as a result, 1) hydrolysis after molecular weight reduce；2) ammonia of peptide side chain
Base is condensed, and reduces amino quantity.Dendritic type is made with formaldehyde condensation reaction in polypeptide and organic nitrogen-containing object, certain
PH under, anion is mutually exclusive between polypeptide, unfolds, and prevents the aggregation of retarder itself, at the same obtain hydrone storage
Space.To reduce unit volume water conservation point under similary retarder dosage, the moisture-holding capacity of increase every, water in guarantor unit's volume
Transmission.Slow setting efficiency is improved, is a practicable technology path.
Invention content
Technical problems based on background technology, the present invention propose a kind of polypeptide condensation resin and prepare gypsum
Retarder.
Technical scheme is as follows：
A kind of preparation method of polypeptide calcium sulphate retarder, includes the following steps：
1) water, organic nitrogen-containing object and formaldehyde are added in the reactor, after stirring evenly, are adjusted with 30% sodium hydroxide solution
PH to 9~11 then heats to 80~90 DEG C, reacts 1~2h, is cooled to 45~55 DEG C, obtains nitrogen methylol condensation product；
2) 45% protein liquid, 30% sodium hydroxide solution is added in into reactor, after stirring evenly, it is desirable that keep pH
To 11~12,70~80 DEG C are then heated to, reacts 0.5~1.5h, pH is adjusted to 9.0~9.5 with 10% sulfuric acid solution, cooling
To 45~55 DEG C, the molecular weight for obtaining degradation polypeptide product is 1500~3000；
3) catabolite in step 2) is added in step 1) nitrogen methylol condensation product, after stirring evenly, with 10% sulfuric acid
Solution adjusts pH to 8.0~9.0, then heats to 60~70 DEG C, reacts 1~2h, then be warming up to 70~75 DEG C, reacts 1~2h,
Be warming up to 80~85 DEG C again, react 1~2h, be cooled to 45~55 DEG C, add in 45~55 DEG C of stirrings 30 of stabilizer and water~
40min obtains the yellow viscous liquid of 300~400mPas.
Preferably, in the step 1), organic nitrogen-containing object can be melamine, dicyandiamide, triaminoguanidine hydrochloride,
The molar ratio of triaminobenzene, organic nitrogen-containing object and formaldehyde is 1:3~3.5..
Preferably, the albumen in the protein liquid be the albumen in the protein liquid be leather discard animal skin glue,
Any one in commercially available industrial gelatine, gelatine.
Preferably, the stabilizer in the step 3) can be dispersing agent NNO L, sodium naphthalene sulfonate, in benzene sulfonic acid formal
Any one, wherein the molar ratio of stabilizer and organic nitrogen-containing object is (0.3~0.5):1, adding water to product solid content is
25%~35%.
Preferably, in the step 3), according to mole of 2000 Molecular weights, wherein catabolite and organic nitrogen-containing object
Than for (2~4):1.
The reaction route of the present invention is schematically as follows：
In above-mentioned signal, R (NH) 2-3 can be in melamine, dicyandiamide, triaminoguanidine hydrochloride, triaminobenzene
Any one.
The invention has the beneficial effects that：Material application result of the present invention has the following advantages that：
1) in terms of setting time and loss of strength two indices, it is excellent that the present invention has that setting time is long, loss of strength is small
Point, three embodiments reach national grade III Standard.
2) it does not add in inorganic salts during materials'use of the present invention, will not lead because stir uneven during production is implemented due to during use
Cause inorganic salts Topical Dispersion is bad to cause crystallization that gypsum is made defect occur.
3) initial set of material of the present invention is approached with final setting time, meets enough process mobility.It can also basis
Blank adjusts the setting time of gypsum with retarder volume.
4) the polypeptide object that the present invention utilizes derives from a wealth of sources, such as leather-making waste Animal Skin and degradation product.
The present invention is based on albumen is hydrophilic and close calcium feature, chemical modification has been carried out to albumen.Utilize polypeptide after degradation and three
Melamine-formaldehyde synthesizes a kind of dendrimer.Since the retarder has good water retaining function, do not crystallized in gypsum, no
It influences gypsum crystal to be formed, final obtain keeps gypsum original intensity good.Embodiment reaches national 3 grades of standard (GB/ of building gypsum
T9776-2008)。
The material of the present invention can be used alone as retarder core material, can also be used as a kind of component and other materials
Material is used in compounding, and still, should also be considered as protection scope of the present invention using the material as in slow setting agent prescription.
Specific embodiment
Retarder synthetic example 1
1) 1 mole of melamine and 3.2 moles of formaldehyde are added in the reactor, add the water of 3 times of melamine quality,
After stirring evenly, pH to 9~11 is adjusted with 30% sodium hydroxide solution, then heats to 80~90 DEG C, react 1~2h, cooling
To 45~55 DEG C, melamine nitrogen methylol condensation product is obtained；
2) 45% hide glue gelatin, 30% sodium hydroxide solution is added in into reactor, after stirring evenly, it is desirable that keep pH
To 11~12,70~80 DEG C are then heated to, reacts 0.5~1.5h, pH is adjusted to 9.0~9.5 with 10% sulfuric acid solution, cooling
To 45~55 DEG C, the molecular weight for obtaining degradation polypeptide product is 1500~3000；
3) by catabolite in step 2) according to 2000 Molecular weights, catabolite:The molar ratio of melamine is 3:1 adds
Enter in step 1) melamine nitrogen methylol condensation product, after stirring evenly, adjust pH to 8.0~9.0 with 10% sulfuric acid solution, so
After be warming up to 60~70 DEG C, react 1~2h, then be warming up to 70~75 DEG C, react 1~2h, then be warming up to 80~85 DEG C, reaction 1
~2h is cooled to 45~55 DEG C, adds in stabilizer (stabilizer:0.4) and 45~55 DEG C of suitable quantity of water the molar ratio of melamine is
30~40min is stirred, it is 25%~35% to obtain solid content, the yellow viscous liquid of 350~400mPas.
Retarder synthetic example 2
1) 1 mole of triaminobenzene and 3.5 moles of formaldehyde are added in the reactor, are added the water of 3 times of triaminobenzene quality, are stirred
After mixing uniformly, pH to 9~11 is adjusted with 30% sodium hydroxide solution, then heats to 80~90 DEG C, 1~2h is reacted, is cooled to
45~55 DEG C, obtain triaminobenzene nitrogen methylol condensation product；
2) 45% gelatin solution, 30% sodium hydroxide solution is added in into reactor, after stirring evenly, it is desirable that keep pH
To 11~12,70~80 DEG C are then heated to, reacts 0.5~1.5h, pH is adjusted to 9.0~9.5 with 10% sulfuric acid solution, cooling
To 45~55 DEG C, the molecular weight for obtaining degradation polypeptide product is 1500~3000；
3) by catabolite in step 2) according to 2000 Molecular weights, catabolite:The molar ratio of triaminobenzene is 3:1 adds
Enter in step 1) triaminobenzene nitrogen methylol condensation product, after stirring evenly, adjust pH to 8.0~9.0 with 10% sulfuric acid solution, so
After be warming up to 60~70 DEG C, react 1~2h, then be warming up to 70~75 DEG C, react 1~2h, then be warming up to 80~85 DEG C, reaction 1
~2h is cooled to 45~55 DEG C, adds in stabilizer (stabilizer:0.3) and 45~55 DEG C of suitable quantity of water the molar ratio of triaminobenzene is
30~40min is stirred, it is 25%~35% to obtain solid content, the yellow viscous liquid of 300~350mPas.
Retarder synthetic example 3
1) 1 mole of triaminoguanidine hydrochloride and 3.5 moles of formaldehyde are added in the reactor, add triaminoguanidine hydrochloride matter
After stirring evenly, pH to 9~11 is adjusted with 30% sodium hydroxide solution, then heats to 80~90 DEG C, reaction 1 for the water of 3 times of amount
~2h is cooled to 45~55 DEG C, obtains triaminoguanidine hydrochloride nitrogen methylol condensation product；
2) 45% gelatin solution, 30% sodium hydroxide solution is added in into reactor, after stirring evenly, it is desirable that keep pH
To 11~12,70~80 DEG C are then heated to, reacts 0.5~1.5h, pH is adjusted to 9.0~9.5 with 10% sulfuric acid solution, cooling
To 45~55 DEG C, the molecular weight for obtaining degradation polypeptide product is 1500~3000；
3) by catabolite in step 2) according to 2000 Molecular weights, catabolite:The molar ratio of triaminoguanidine hydrochloride
It is 3:1 adds in step 1) triaminoguanidine hydrochloride nitrogen methylol condensation product, and after stirring evenly, pH is adjusted with 10% sulfuric acid solution
To 8.0~9.0,60~70 DEG C are then heated to, reacts 1~2h, then be warming up to 70~75 DEG C, reacts 1~2h, then be warming up to 80
~85 DEG C, 1~2h is reacted, is cooled to 45~55 DEG C, adds in stabilizer (stabilizer:The molar ratio of triaminoguanidine hydrochloride is
0.4) and 45~55 DEG C of suitable quantity of water stirs 30~40min, and it is 25%~35% to obtain solid content, the yellow of 350~350mPas
Viscous liquid.
Retarder Application Example
The addition of retarder is 0.2% (mass fraction) of gypsum quality, and the thick water requirement of gypsum mark is 0.50, according to building
It builds gypsum GB/T 9776-2008 and carries out setting time, strength character test, it is as a result as shown in table 1 below.
1 building gypsum physical and mechanical property of table
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (6)
1. a kind of preparation method of polypeptide calcium sulphate retarder, which is characterized in that include the following steps：
1) water, organic nitrogen-containing object and formaldehyde are added in the reactor, after stirring evenly, with 30% sodium hydroxide solution adjust pH to
9~11,80~90 DEG C are then heated to, reacts 1~2h, is cooled to 45~55 DEG C, obtains nitrogen methylol condensation product；
2) 45% protein liquid, 30% sodium hydroxide solution is added in into reactor, after stirring evenly, it is desirable that keep pH to 11
~12,70~80 DEG C are then heated to, 0.5~1.5h is reacted, pH is adjusted to 9.0~9.5 with 10% sulfuric acid solution, is cooled to 45
~55 DEG C, the molecular weight for obtaining degradation polypeptide product is 1500~3000；
3) catabolite in step 2) is added in step 1) nitrogen methylol condensation product, after stirring evenly, with 10% sulfuric acid solution
PH to 8.0~9.0 is adjusted, then heats to 60~70 DEG C, reacts 1~2h, then be warming up to 70~75 DEG C, reacts 1~2h, then rise
Temperature reacts 1~2h to 80~85 DEG C, is cooled to 45~55 DEG C, adds in 45~55 DEG C of 30~40min of stirring of stabilizer and water, obtains
Obtain the yellow viscous liquid of 300~400mPas.
2. the preparation method of polypeptide calcium sulphate retarder as described in claim 1, which is characterized in that the step 1)
In, organic nitrogen-containing object can be melamine, dicyandiamide, triaminoguanidine hydrochloride, triaminobenzene, organic nitrogen-containing object and formaldehyde
Molar ratio is 1:3~3.5.
3. the preparation method of polypeptide calcium sulphate retarder as described in claim 1, which is characterized in that in the protein liquid
Albumen be that leather discards any one in animal skin glue, commercially available industrial gelatine, gelatine.
4. the preparation method of polypeptide calcium sulphate retarder as described in claim 1, which is characterized in that in the step 3)
Stabilizer can be dispersing agent NNO L, sodium naphthalene sulfonate, any one in benzene sulfonic acid formal, wherein stabilizer contains with organic
The molar ratio of nitrogen object is (0.3~0.5):1, it is 25%~35% to add water to product solid content.
5. the preparation method of polypeptide calcium sulphate retarder as claimed in claim 4, which is characterized in that the step 3)
In, according to 2000 Molecular weights, the molar ratio of wherein catabolite and organic nitrogen-containing object is (3~4):1.
6. a kind of polypeptide gypsum according to obtained by claim 1-5 any material proportion compositions, process delays
Solidifying agent.
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| CN201810069496.6A CN108249792B (en) | 2018-01-24 | 2018-01-24 | Preparation method of protein polypeptide gypsum retarder |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112028526A (en) * | 2020-09-14 | 2020-12-04 | 泰山石膏有限公司 | Gypsum retarder and preparation method and application thereof |
| CN115678034A (en) * | 2022-10-14 | 2023-02-03 | 海南太和科技有限公司 | Modified plant hydrolyzed protein retarder as well as preparation method and application thereof |
| CN117567066A (en) * | 2024-01-16 | 2024-02-20 | 申辉(河北)精化有限责任公司 | Modified protein polypeptide-based gypsum retarder and preparation method thereof |
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| CN107098667A (en) * | 2017-06-28 | 2017-08-29 | 武汉菡美洛建筑材料有限公司 | Gypsum base light energy conservation plate and preparation method thereof |
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| JP2001261395A (en) * | 2000-03-16 | 2001-09-26 | Ajinomoto Co Inc | Setting retarder for gypsum |
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| CN104086115A (en) * | 2014-07-14 | 2014-10-08 | 广东龙湖科技股份有限公司 | Gypsum retarder capable of improving strength and binding strength of gypsum base material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112028526A (en) * | 2020-09-14 | 2020-12-04 | 泰山石膏有限公司 | Gypsum retarder and preparation method and application thereof |
| CN115678034A (en) * | 2022-10-14 | 2023-02-03 | 海南太和科技有限公司 | Modified plant hydrolyzed protein retarder as well as preparation method and application thereof |
| CN115678034B (en) * | 2022-10-14 | 2024-04-19 | 海南太和科技有限公司 | Modified plant hydrolyzed protein retarder and preparation method and application thereof |
| CN117567066A (en) * | 2024-01-16 | 2024-02-20 | 申辉(河北)精化有限责任公司 | Modified protein polypeptide-based gypsum retarder and preparation method thereof |
| CN117567066B (en) * | 2024-01-16 | 2024-03-22 | 申辉(河北)精化有限责任公司 | Modified protein polypeptide-based gypsum retarder and preparation method thereof |
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