CN115626791B - Nano calcium enhanced additive, resin and artificial granite - Google Patents

Nano calcium enhanced additive, resin and artificial granite Download PDF

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CN115626791B
CN115626791B CN202211362761.2A CN202211362761A CN115626791B CN 115626791 B CN115626791 B CN 115626791B CN 202211362761 A CN202211362761 A CN 202211362761A CN 115626791 B CN115626791 B CN 115626791B
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parts
nano
calcium
nano calcium
powder
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CN115626791A (en
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黄安定
王安东
王钰馨
陈海生
朱勇
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Shaanxi Andong Xingyang Gangshi Technology Co ltd
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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
    • C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
    • C04B40/0028—Aspects relating to the mixing step of the mortar preparation
    • C04B40/0039—Premixtures of ingredients
    • C04B40/0046—Premixtures of ingredients characterised by their processing, e.g. sequence of mixing the ingredients when preparing the premixtures
    • 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
    • C04B24/34—Natural resins, e.g. rosin
    • 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
    • C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
    • C04B26/02—Macromolecular compounds
    • C04B26/10—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B26/18—Polyesters; Polycarbonates
    • 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
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/54—Substitutes for natural stone, artistic materials or the like
    • C04B2111/542—Artificial natural stone
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/91—Use of waste materials as fillers for mortars or concrete

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Macromonomer-Based Addition Polymer (AREA)

Abstract

The invention discloses a nano calcium enhanced additive which is prepared from the following raw materials in parts by weight: 100 parts of nano calcium powder, 1-5 parts of oleic acid, 2-5 parts of methyl ethyl ketone peroxide, 2-5 parts of di-tert-butyl diisopropyl peroxide, 5-10 parts of rosin powder, 5-25 parts of methyl methacrylate and 5-50 parts of styrene/N-vinyl pyrrolidone. The invention also discloses a nano calcium reinforced resin, which comprises the additive. The invention also discloses a nano calcium enhanced artificial granite, which comprises the nano calcium enhanced resin. The invention can solve the problems of long time consumption in the process of mixing artificial stone materials and insufficient contact between UPR and aggregate caused by high viscosity and large usage amount of UPR in the prior art.

Description

Nano calcium enhanced additive, resin and artificial granite
Technical Field
The invention belongs to the field of artificial granite preparation, and particularly relates to a nano calcium enhanced additive, resin and artificial granite.
Background
The artificial granite is also called artificial marble, and is made up by using crushed aggregates and powder of carbonate stone (marble and limestone, etc.) as main filler, adding adhesive, various fillers and pigments, curing agent and auxiliary agent of initiator, etc., and making them pass through the processes of stirring, forming, curing, cutting and polishing.
The artificial granite in the market at present is mostly Unsaturated Polyester (UPR) based artificial granite, namely unsaturated polyester is used as a binder.
Chinese patent CN114262172a discloses a pretreatment agent and pretreatment method for artificial granite raw material, which comprises the following components in parts by mass: 1 to 5 parts of activating agent and 0.5 to 3 parts of cross-linking agent; the activating agent comprises the following components in parts by mass: 45-60 parts of styrene, 5-15 parts of silane coupling agent, 5-10 parts of chelate titanate, 5-10 parts of acrylamide and 5-15 parts of unsaturated polyester resin; the cross-linking agent comprises the following components in parts by mass: 60 to 90.995 parts of styrene, 5 to 35 parts of unsaturated polyester resin and 0.1 to 0.5 part of azodiisobutyronitrile. The pretreatment agent is adopted to pretreat the artificial granite aggregate, the activating agent is added into the artificial granite aggregate at one time to be fully stirred, then the cross-linking agent is slowly added into the artificial granite aggregate to be fully stirred, and then the artificial granite aggregate is produced into the artificial granite product according to the conventional process. The invention can reduce the resin consumption, thereby reducing the production cost.
Chinese patent CN113929360a discloses a water-mark beige artificial granite, wherein the raw materials include calcium carbonate coarse sand, superfine calcium carbonate powder, lemon yellow powder, titanium pigment, water, unsaturated polyester resin, glycerol, sodium carboxymethyl cellulose, polyethylene oxide, carboxymethyl chitosan, vinyl versatate, polydimethylsiloxane, magnesium aluminum silicate, nano silica, curing agent and accelerator; the invention prepares the raw materials in the formula into base material, color paste, surface material, base material, mixed solution A and slurry B respectively, prepares the base material, color paste, base material, mixed solution A and slurry B into blank by curing agent and accelerator, distributes the surface material onto the blank, and obtains the water-grain beige artificial granite with good impact resistance, high bending strength, good acid and alkali resistance and good pollution resistance by curing molding, demoulding, normal temperature and normal pressure maintenance, cutting and flat grinding.
Chinese patent CN113233819a discloses a natural crack imitation artificial granite, wherein the raw materials include: calcium carbonate coarse sand, superfine calcium carbonate powder, unsaturated polyester resin, toner, titanium pigment, methyl ethyl ketone peroxide, cobalt isooctanoate, a coupling agent, styrene, stearic acid, sodium phenylpropionate and glycerol; the composite acid modification is produced by using the octadecanoic acid and the sodium benzoate, then the composite acid modification is added by matching with the glycerol and the styrene according to the ratio, the unsaturated acid content in the unsaturated polyester resin is reduced, the shock resistance of the unsaturated polyester resin is improved, the cracking condition of the artificial stone in the production process is reduced, the defective rate of the artificial stone product is reduced, the base material is scattered into a mould paved with auxiliary materials through a cloth machine, the auxiliary materials and the base material in the mould are subjected to vibration press molding through the artificial stone vibration molding machine to form an artificial stone blank with natural-imitated cracks, different crack patterns are presented on the artificial stone blank, and the appearance diversity of the artificial stone is improved.
The invention discloses a preparation method of low-resin multicolor granite, which comprises the following raw materials (based on the total amount of the raw materials): 20 to 40 percent of calcium carbonate (90 meshes), 40 to 60 percent of calcium carbonate (400 meshes), 3 to 9 percent of superfine barium sulfate (1000 to 2000 meshes), 7 to 9 percent of unsaturated polyester resin, 1 to 3 percent of curing agent (based on the weight of the unsaturated polyester resin), 0.01 to 0.3 percent of accelerator (based on the weight of the unsaturated polyester resin), 3 to 6 percent of volatile diluent (based on the weight of the unsaturated polyester resin), 0 to 0.3 percent of pigment, and the like. The unsaturated polyester resin dosage of the multicolor sentry stone is reduced by 5-10% in a breakthrough manner, and the expansion coefficient of the multicolor sentry stone is reduced, so that the multicolor sentry stone has low shrinkage and wear resistance, the quality is improved, and meanwhile, the production cost of the multicolor sentry stone is reduced, the market prospect is wide, and the multicolor sentry stone has good economic and social benefits.
The method mainly aims at the compounding treatment of the granite aggregate and the like, does not aim at UPR, and cannot solve the defects of high viscosity of UPR, difficult mixing process, difficult mixing of aggregate and the like in practical production and application.
Disclosure of Invention
The invention aims to provide a nano calcium enhanced additive, which solves the problems of long time consumption in the process of mixing artificial stone and insufficient contact between UPR and aggregate caused by high viscosity and large usage amount of UPR in the prior art.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the nano calcium enhanced additive is prepared from the following raw materials in parts by weight: 100 parts of nano calcium powder, 1-5 parts of oleic acid, 2-5 parts of methyl ethyl ketone peroxide, 2-5 parts of di-tert-butyl diisopropyl peroxide, 5-10 parts of rosin powder, 5-25 parts of methyl methacrylate and 5-50 parts of styrene/N-vinyl pyrrolidone.
Further, the preparation method of the nano calcium enhanced additive comprises the following steps:
A. taking nano calcium powder, and placing the nano calcium powder in a 105 ℃ drying oven for full drying for later use;
B. mixing oleic acid, methyl ethyl ketone oxide, di-tert-butyl diisopropyl benzene peroxide, rosin powder, methyl methacrylate and nano calcium powder at room temperature under stirring, and adding styrene/N-vinyl pyrrolidone to obtain a thin paste.
The invention also provides a nano calcium reinforced resin which comprises the additive and 600-700 parts of unsaturated polyester resin.
Further, the preparation method of the nano calcium reinforced resin comprises the following steps: and mixing and stirring the unsaturated polyester resin and the additive uniformly to obtain the polyester resin.
Further, the stirring rate is 100-500 r/min.
Further, the stirring time is 5-10 min.
The invention also provides the nano calcium reinforced artificial granite, which is applied to the nano calcium reinforced resin and also comprises conventional artificial stone aggregate.
Further, the artificial stone aggregate is 5000-6500 parts, and the nano calcium reinforced resin is 550-850 parts.
Further, the preparation method of the nano calcium enhanced artificial granite comprises the following steps: adding nano calcium reinforced resin into conventional artificial stone aggregate, fully mixing, pressing, and curing for 45-75 min to obtain the artificial stone.
Further, the curing temperature was 90 ℃.
In the invention, the structural formula of oleic acid is as follows:
Figure BDA0003923312380000041
the main component abietic acid-structural formula of rosin is as follows:
Figure BDA0003923312380000051
methyl methacrylate has the structural formula:
Figure BDA0003923312380000052
the structural formula of the styrene is as follows:
Figure BDA0003923312380000053
the N-vinyl pyrrolidone has the following structural formula:
Figure BDA0003923312380000061
the invention has the following action mechanism and beneficial effects:
1. according to the invention, oleic acid, rosin, methyl methacrylate and styrene are used as monomers with double bonds in a compounding way, methyl ethyl ketone peroxide is used as an initiator, di-tert-butyl diisopropyl peroxide is used as a cross-linking agent, double bonds in each monomer are promoted to be opened in a system, bonding and cross-linking are performed, a space structure which is more diversified and complicated than that in the original resin curing process is formed under a proper proportioning condition, and dispersed nano calcium is used as a core point in the structure, so that the strength of the resin after curing is further improved, and the resin with more excellent comprehensive strength is formed.
2. According to the invention, a small amount of nano calcium loaded curing agent, cross-linking agent and vinyl monomer are utilized to directly carry out mixing modification treatment on UPR resin, so that the viscosity of UPR itself can be effectively reduced, the time consumption of the artificial stone mixing process is shortened, and the UPR and aggregate are fully contacted and fused; the nano calcium loaded partial curing agent, the cross-linking agent and the vinyl monomer can be fully dispersed in the UPR, and no auxiliary agents such as the curing agent and the like are required to be added separately in the subsequent flow, so that the process is simplified.
3. The nano calcium of the invention has consistent components with the aggregate of the artificial stone, does not have negative effects, and can be directly dispersed as rigid particles to act on UPR resin to play a certain role in reinforcing, reduce UPR usage amount, save production cost and maintain or even strengthen the mechanical strength of the artificial stone product.
Detailed Description
For a better understanding of the present invention, reference is made to the following examples, which are included within the scope of the present invention, but are not intended to limit the scope of the present invention.
Example 1
The preparation method of the nano calcium enhanced additive comprises the following steps:
A. taking 100 parts of nano calcium powder, and placing the powder in a 105 ℃ drying oven for full drying for later use;
B. mixing 1 part of oleic acid, 3 parts of methyl ethyl ketone oxide, 5 parts of di-tert-butyl diisopropyl benzene peroxide, 5 parts of rosin powder, 10 parts of methyl methacrylate and nano calcium powder at room temperature under stirring, and continuously adding 5 parts of styrene/N-vinyl pyrrolidone to be regulated into a thin paste.
A preparation method of nano calcium reinforced resin comprises the following steps: mixing the additive thin paste with 600 parts of unsaturated polyester resin, and stirring for 5min at the speed of 500r/min.
The preparation method of the artificial granite comprises the following steps: 5000 parts of conventional artificial stone aggregate is taken, 550 parts of nano calcium reinforced resin is added, the mixture is fully mixed and then pressed, and the mixture is cured for 45 minutes at 90 ℃ to obtain the artificial granite.
Example 2
The preparation method of the nano calcium enhanced additive comprises the following steps:
A. taking 100 parts of nano calcium powder, and placing the powder in a 105 ℃ drying oven for full drying for later use;
B. 2 parts of oleic acid, 2 parts of methyl ethyl ketone oxide, 2 parts of di-tert-butyl diisopropyl benzene peroxide, 6 parts of rosin powder, 5 parts of methyl methacrylate and nano calcium powder are fully stirred and mixed at room temperature, and then 10 parts of styrene/N-vinyl pyrrolidone is continuously added to be regulated into a thin paste.
A preparation method of nano calcium reinforced resin comprises the following steps: mixing the additive thin paste with 700 parts of unsaturated polyester resin, and stirring for 8min at the speed of 300 r/min.
The preparation method of the artificial granite comprises the following steps: 5500 parts of conventional artificial stone aggregate is taken, 600 parts of nano calcium reinforced resin is added, the mixture is fully mixed and then pressed, and the mixture is cured for 50 minutes at 90 ℃ to obtain the artificial granite.
Example 3
The preparation method of the nano calcium enhanced additive comprises the following steps:
A. taking 100 parts of nano calcium powder, and placing the powder in a 105 ℃ drying oven for full drying for later use;
B. mixing 3 parts of oleic acid, 4 parts of methyl ethyl ketone oxide, 3 parts of di-tert-butyl diisopropyl peroxide, 7 parts of rosin powder, 10 parts of methyl methacrylate and nano calcium powder at room temperature, and continuously adding 25 parts of styrene/N-vinyl pyrrolidone to adjust to be in a thin paste state.
A preparation method of nano calcium reinforced resin comprises the following steps: mixing the additive thin paste with 650 parts of unsaturated polyester resin, and stirring for 10min at the speed of 250 r/min.
The preparation method of the artificial granite comprises the following steps: taking 5200 parts of conventional artificial stone aggregate, adding 650 parts of nano calcium reinforced resin, fully mixing, pressing, and curing at 90 ℃ for 65min to obtain the artificial granite.
Example 4
The preparation method of the nano calcium enhanced additive comprises the following steps:
A. taking 100 parts of nano calcium powder, and placing the powder in a 105 ℃ drying oven for full drying for later use;
B. 4 parts of oleic acid, 5 parts of methyl ethyl ketone oxide, 4 parts of di-tert-butyl diisopropyl benzene peroxide, 9 parts of rosin powder, 15 parts of methyl methacrylate and nano calcium powder are fully stirred and mixed at room temperature, and then 30 parts of styrene/N-vinyl pyrrolidone are continuously added to be regulated into a thin paste.
A preparation method of nano calcium reinforced resin comprises the following steps: mixing the additive thin paste with 700 parts of unsaturated polyester resin, and stirring for 10min at the speed of 100 r/min.
The preparation method of the artificial granite comprises the following steps: 5800 parts of conventional artificial stone aggregate is taken, 800 parts of nano calcium reinforced resin is added, the mixture is fully mixed and then pressed, and the mixture is cured for 70 minutes at 90 ℃ to obtain the artificial granite.
Example 5
The preparation method of the nano calcium enhanced additive comprises the following steps:
A. taking 100 parts of nano calcium powder, and placing the powder in a 105 ℃ drying oven for full drying for later use;
B. mixing 5 parts of oleic acid, 5 parts of methyl ethyl ketone oxide, 2 parts of di-tert-butyl diisopropyl benzene peroxide, 10 parts of rosin powder, 25 parts of methyl methacrylate and nano calcium powder at room temperature under stirring, and continuously adding 50 parts of styrene/N-vinyl pyrrolidone to be regulated into a thin paste.
A preparation method of nano calcium reinforced resin comprises the following steps: mixing the additive thin paste with 600 parts of unsaturated polyester resin, and stirring for 6min at the speed of 500r/min.
The preparation method of the artificial granite comprises the following steps: 6500 parts of conventional artificial stone aggregate is taken, 850 parts of nano calcium reinforced resin is added, the mixture is fully mixed and pressed, and the mixture is cured for 75 minutes at 90 ℃ to obtain the artificial granite.
Comparative example 1
Substantially the same as in example 3, except that rosin powder, methyl methacrylate, styrene were not contained in the raw materials for preparation.
Comparative example 2
Substantially the same as in example 3, except that oleic acid, methyl methacrylate and styrene were not contained in the raw materials for production.
Comparative example 3
Substantially the same as in example 3, except that oleic acid, rosin powder, and styrene were not contained in the raw materials for preparation.
Comparative example 4
Substantially the same as in example 3, except that oleic acid, rosin powder, methyl methacrylate were not contained in the raw materials for preparation.
Comparative example 5
Substantially the same as in example 3, except that oleic acid, rosin powder, methyl methacrylate, styrene were not contained in the raw materials for preparation.
Performance comparison experiment
Artificial granite is prepared according to the methods of examples 1-5 and comparative examples 1-5, 7 standard samples are taken from each group, the bending strength and the compressive strength are measured according to GB/T35157-2017 resin type synthetic stone slabs, and the average value of the test results is obtained.
The test results are shown in the following table:
Figure BDA0003923312380000101
Figure BDA0003923312380000111
from the above table, it can be seen that:
the artificial granite prepared in the invention of examples 1-5 has higher flexural strength and compressive strength, wherein example 3 is the most preferred example.
Comparative example 5 does not contain oleic acid, rosin powder, methyl methacrylate, and styrene, and the bending strength and the compressive strength are significantly reduced as compared with example 3. The comparative examples 1 to 4 can improve the bending strength and the compression strength to a certain extent by adding oleic acid, rosin powder, methyl methacrylate and styrene on the basis of the comparative example 5 respectively, but the total improvement amount of the four components is still lower than that of the comparative example 5 compared with the example 3.
When oleic acid is a long carbon chain, methyl methacrylate and abietic acid, styrene or other monomers with benzene rings or cyclic carbon chains coexist, nano calcium can be used as a core connection point, di-tert-butyl diisopropyl peroxide is used as a cross-linking agent, double bonds in the monomers are promoted to be opened in a system, bonding and cross-linking are carried out, a space structure which is more diversified and complicated than that in the original resin curing process is formed under the condition of proper proportion, and the structure can synergistically improve the strength of the cured resin after curing, so that the cured resin with more excellent comprehensive strength is formed.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (9)

1. The nano calcium enhanced additive is characterized by being prepared from the following raw materials in parts by weight: 100 parts of nano calcium powder, 1-5 parts of oleic acid, 2-5 parts of methyl ethyl ketone peroxide, 2-5 parts of di-tert-butyl diisopropyl benzene peroxide, 5-10 parts of rosin powder, 5-25 parts of methyl methacrylate and 5-50 parts of styrene/N-vinyl pyrrolidone;
the preparation method of the nano calcium enhanced additive comprises the following steps:
A. taking nano calcium powder, and placing the nano calcium powder in a 105 ℃ drying oven for full drying for later use;
B. mixing oleic acid, methyl ethyl ketone oxide, di-tert-butyl diisopropyl benzene peroxide, rosin powder, methyl methacrylate and nano calcium powder at room temperature under stirring, and adding styrene/N-vinyl pyrrolidone to obtain a thin paste.
2. The nano-calcium reinforced resin is characterized by comprising the additive according to claim 1 and 600-700 parts of unsaturated polyester resin.
3. The nano-calcium reinforced resin according to claim 2, wherein the preparation method comprises the following steps: and mixing and stirring the unsaturated polyester resin and the additive uniformly to obtain the polyester resin.
4. A nano-calcium reinforced resin according to claim 3, characterized in that: the stirring speed is 100-500 r/min.
5. A nano-calcium reinforced resin according to claim 3, characterized in that: the stirring time is 5-10 min.
6. A nano-calcium enhanced artificial granite, wherein the nano-calcium enhanced resin according to any of claims 2-5 is applied, and further comprising artificial stone aggregate.
7. The nano-calcium enhanced artificial granite according to claim 6, wherein: 5000-6500 parts of artificial stone aggregate and 550-850 parts of nano calcium reinforced resin.
8. The nano-calcium enhanced artificial granite according to claim 6, wherein the preparation method is as follows: and adding nano calcium reinforced resin into the artificial stone aggregate, fully mixing, pressing, and curing for 45-75 min to obtain the artificial stone.
9. The nano-calcium enhanced artificial granite according to claim 7, wherein: the curing temperature was 90 ℃.
CN202211362761.2A 2022-11-02 2022-11-02 Nano calcium enhanced additive, resin and artificial granite Active CN115626791B (en)

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Publication number Priority date Publication date Assignee Title
CN101555308B (en) * 2008-11-06 2011-09-28 常州市华润复合材料有限公司 Unsaturated polyester resin for alpine rock
CN111592667B (en) * 2020-06-01 2021-07-13 广西科学院 Reinforced antibacterial artificial granite waste residue-based plastic master batch and preparation method thereof
CN113233819A (en) * 2021-06-21 2021-08-10 广东省宝云石业有限公司 Artificial granite with natural crack and production process thereof
CN114262172B (en) * 2021-11-20 2023-01-24 广西科学院 Pretreatment agent and pretreatment method for artificial granite raw material

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