CN109943239B - Preparation method of nontoxic tissue slice mounting adhesive - Google Patents
Preparation method of nontoxic tissue slice mounting adhesive Download PDFInfo
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- CN109943239B CN109943239B CN201711392664.7A CN201711392664A CN109943239B CN 109943239 B CN109943239 B CN 109943239B CN 201711392664 A CN201711392664 A CN 201711392664A CN 109943239 B CN109943239 B CN 109943239B
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Abstract
The invention discloses a preparation method of nontoxic tissue slice mounting glue, and belongs to the technical field of tissue slice preparation. Mixing isooctyl polymethacrylate mixed glue, limonene and fir glue to obtain mounting glue; the isooctyl polymethacrylate mixed glue is prepared from isooctyl methacrylate, D30 solvent oil and a guiding agent. The raw materials used by the method are low in price and easy to obtain, do not contain toxic and harmful substances, are environment-friendly, and the mounting adhesive prepared by the method is low in taste, free of irritation, excellent in refractive index, quick to dry, excellent in hardness and toughness, very good in mounting effect, and suitable for preparing the mounting adhesive.
Description
Technical Field
The invention relates to a preparation method of nontoxic tissue slice mounting glue, belonging to the technical field of pathological tissue slice preparation.
Background
In the field of preparation of tissue sections for medical pathological diagnosis, final mounting of mounting glue is required. The sealing glue in the market has various types, such as pure plant extracted Canadian fir glue, synthesized neutral resin glue and other glue synthesized by taking dimethylbenzene as a solvent. Although the Canadian fir glue is non-toxic and environment-friendly, the Canadian fir glue is expensive, has unsatisfactory refractive index, slow drying speed and low hardness after drying, and is easy to shift a cover glass of a tissue mounting piece during observation to influence the microscopic observation after mounting; other commercially available synthetic film sealants contain either xylene, which is a hazardous substance, or aromatic rings, ammonia, sulfur, and other chemicals that are unpleasant in taste and harmful to health.
Disclosure of Invention
In order to solve the problems that the prior mounting adhesive is high in price, contains toxic and harmful substances, has poor refractive index, slow drying speed and low hardness after drying, easily displaces a tissue mounting cover glass during observation and influences microscope observation after mounting, the invention provides a preparation method of the non-toxic tissue slice mounting adhesive, the mounting adhesive is non-toxic and environment-friendly (does not contain the toxic and harmful substances), the raw materials are easy to purchase, the price is low, the taste is low, the irritation is low, the refractive index is excellent, the quick drying property is high, and the hardness is high, and the adopted technical scheme is as follows:
the invention aims to provide a preparation method of nontoxic tissue slice mounting glue, which is characterized in that isooctyl polymethacrylate mixed glue, limonene and fir glue are mixed at normal temperature to obtain mounting glue; the mixed glue of the isooctyl methacrylate is prepared by isooctyl methacrylate, D30 solvent oil and a guiding agent (benzoyl peroxide or azodiisobutyronitrile).
Preferably, the preparation method comprises the steps of mixing 85-96 parts by weight of isooctyl methacrylate mixed glue, 2-5 parts by weight of limonene and 2-10 parts by weight of fir glue to obtain the mounting glue; the mixed glue of the isooctyl methacrylate is prepared by 50 to 60 weight parts of isooctyl methacrylate, 40 to 50 weight parts of D30 solvent oil and 0.9 to 1.5 weight parts of guiding agent (benzoyl peroxide or azobisisobutyronitrile).
More preferably, the preparation method comprises the steps of mixing 90-93 parts by weight of isooctyl methacrylate mixed glue, 3-4 parts by weight of limonene and 4-6 parts by weight of fir glue to obtain the mounting glue; the isooctyl methacrylate mixed glue is prepared from 54-58 parts by weight of isooctyl methacrylate, 42-46 parts by weight of D30 solvent oil and 1.14-1.38 parts by weight of guiding agent.
More preferably, the preparation method comprises the steps of mixing 92 parts by weight of isooctyl polymethacrylate mixed glue, 3 parts by weight of limonene and 5 parts by weight of fir glue to obtain a mounting glue; the isooctyl methacrylate mixed glue is prepared from 55 parts by weight of isooctyl methacrylate, 45 parts by weight of D30 solvent oil and 1.2 parts by weight of guiding agent.
Preferably, the guiding agent is benzoyl peroxide or azobisisobutyronitrile, which can achieve better effects, especially benzoyl peroxide.
Preferably, the preparation method of the isooctyl polymethacrylate mixed sol comprises the following steps:
1) initial polymerization reaction: fully and uniformly mixing isooctyl methacrylate and D30 solvent oil by 100 parts by weight, adding the mixture into a reaction kettle, continuously stirring the mixture, controlling the stirring speed of a stirring paddle to be 120r/min, controlling the temperature to be 110-120 ℃, then adding 0.1 part by weight of guiding agent every 10min, controlling the total adding amount of the guiding agent to be 0.3 part by weight, and carrying out primary polymerization for 30 min;
2) and (3) repolymerization: and continuously heating the primary polymerization reactant to 140-145 ℃, preserving the heat, continuously stirring, adding 0.1-0.2 part by weight of the guiding agent into the mixture every 20min at the stirring speed of 120r/min for 6 times, preserving the heat and reacting for 40min, and finishing the polymerization reaction.
Further, the addition amount of the guiding agent in the step 2) is as follows: 0.14 to 0.18 parts by weight of the additive is added every 20min for 6 times in total.
The invention has the beneficial effects that:
the invention provides a preparation method of a novel sealing adhesive, the raw materials used in the method are cheap and easy to obtain, toxic and harmful substances are not contained, the method is environment-friendly, and the sealing adhesive prepared by the method has no pungent smell, excellent refractive index, quick drying, large hardness and very good sealing effect.
The invention provides a preparation method of isooctyl methacrylate mixed glue, which is characterized in that isooctyl methacrylate, D30 solvent oil and a guiding agent are used for carrying out self-polymerization reaction on isooctyl methacrylate, thereby preparing the isooctyl methacrylate mixed glue.
In the invention, D30 is added into the self-polymerization reaction of isooctyl methacrylate to play a role of excellent dissolving diluent; the isooctyl polymethacrylate is a main component of the mounting adhesive and provides an adhesive effect; the limonene plays a role of a diluting and dissolving agent of the isooctyl methacrylate; the fir rubber can overcome the defects that the isooctyl polymethacrylate is too hard and the toughness is poor, so that the sealing piece rubber has excellent hardness and toughness.
Detailed Description
The present invention will be further described with reference to the following specific examples, but the present invention is not limited to these examples.
Example 1
The embodiment provides a preparation method of nontoxic tissue slice mounting glue, which comprises the following steps: and fully mixing 96 parts by weight of isooctyl polymethacrylate mixed glue, 2 parts by weight of limonene and 2 parts by weight of fir glue at normal temperature to obtain the mounting glue.
The mixed glue of the isooctyl methacrylate is prepared by 50 weight parts of isooctyl methacrylate, 50 weight parts of D30 solvent oil and 0.9 weight part of guiding agent (benzoyl peroxide), and the specific preparation method of the mixed glue of the isooctyl methacrylate is as follows:
(1) initial polymerization reaction: fully and uniformly mixing 50 parts by weight of isooctyl methacrylate and 50 parts by weight of D30 solvent oil at normal temperature, adding the mixture into a reaction kettle, continuously stirring the mixture at the stirring speed of 120r/min, controlling the temperature to be 110-120 ℃, then adding 0.1 part by weight of guiding agent into the mixture every 10min, controlling the total adding amount of the guiding agent to be 0.3 part by weight, and carrying out initial polymerization for 30 min;
(2) and (3) repolymerization: and continuously heating the primary polymerization reaction product to 140-145 ℃, continuously stirring at the stirring speed of 120r/min, preserving the heat, adding 0.1 part by weight of the guiding agent every 20min, adding for 6 times in total, preserving the heat, reacting for 40min, and finishing the polymerization reaction.
Example 2
The embodiment provides a preparation method of nontoxic tissue slice mounting glue, which comprises the following steps: and fully mixing 92 parts by weight of isooctyl polymethacrylate mixed glue, 3 parts by weight of limonene and 5 parts by weight of fir glue at normal temperature to obtain the mounting glue.
The mixed glue of the isooctyl methacrylate is prepared by 55 weight parts of isooctyl methacrylate, 45 weight parts of D30 solvent oil and 1.2 weight parts of guiding agent (benzoyl peroxide), and the specific preparation method of the mixed glue of the isooctyl methacrylate is as follows:
(1) initial polymerization reaction: fully and uniformly mixing 55 parts by weight of isooctyl methacrylate and 45 parts by weight of D30 solvent oil at normal temperature, adding the mixture into a reaction kettle, controlling the temperature to be 110-120 ℃, continuously stirring at the stirring speed of 120r/min, then adding 0.1 part by weight of guiding agent every 10min, controlling the total addition of the guiding agent to be 0.3 part by weight, and carrying out initial polymerization for 30 min;
(2) and (3) repolymerization: and continuously heating the primary polymerization reaction product to 140-145 ℃, preserving heat, continuously stirring at the stirring speed of 120r/min, adding 0.15 part by weight of the guiding agent every 20min for 6 times, preserving heat and reacting for 40min, and finishing the polymerization reaction.
Example 3
The embodiment provides a preparation method of nontoxic tissue slice mounting glue, which comprises the following steps: and fully mixing 90 parts by weight of isooctyl polymethacrylate mixed glue, 4 parts by weight of limonene and 6 parts by weight of fir glue at normal temperature to obtain the mounting glue.
The mixed glue of the isooctyl methacrylate is prepared by 55 weight parts of isooctyl methacrylate, 45 weight parts of D30 solvent oil and 1.5 weight parts of guiding agent (benzoyl peroxide), and the specific preparation method of the mixed glue of the isooctyl methacrylate is as follows:
(1) initial polymerization reaction: fully and uniformly mixing 55 parts by weight of isooctyl methacrylate and 45 parts by weight of D30 solvent oil at normal temperature, adding the mixture into a reaction kettle, controlling the temperature to be 110-120 ℃, continuously stirring at the stirring speed of 120r/min, then adding 0.1 part by weight of guiding agent every 10min, controlling the total addition of the guiding agent to be 0.3 part by weight, and carrying out initial polymerization for 30 min;
(2) and (3) repolymerization: and continuously heating the primary polymerization reaction product to 140-145 ℃, preserving the heat, continuously stirring at the stirring speed of 120r/min, adding 0.2 part by weight of guiding agent (benzoyl peroxide) every 20min, adding for 6 times, preserving the heat, reacting for 40min, and finishing the polymerization reaction.
Example 4
The embodiment provides a preparation method of nontoxic tissue slice mounting glue, which comprises the following steps: and fully mixing 87 parts by weight of isooctyl polymethacrylate mixed glue, 5 parts by weight of limonene and 8 parts by weight of fir glue at normal temperature to obtain the mounting glue.
The isooctyl methacrylate mixed glue is prepared from 57 parts by weight of isooctyl methacrylate, 43 parts by weight of D30 solvent oil and 1.14 parts by weight of guiding agent (benzoyl peroxide), and the specific preparation method of the isooctyl methacrylate mixed glue is as follows:
(1) initial polymerization reaction: fully and uniformly mixing 57 parts by weight of isooctyl methacrylate and 43 parts by weight of D30 solvent oil at normal temperature, adding the mixture into a reaction kettle, controlling the temperature to be 110-120 ℃, continuously stirring at the stirring speed of 120r/min, then adding 0.1 part by weight of guiding agent every 10min, controlling the total addition of the guiding agent to be 0.3 part by weight, and carrying out primary polymerization for 30 min;
(2) and (3) repolymerization: and continuously heating the primary polymerization reaction product to 140-145 ℃, preserving heat, continuously stirring at the stirring speed of 120r/min, adding 0.14 part by weight of the guiding agent every 20min for 6 times, preserving heat and reacting for 40min, and finishing the polymerization reaction.
Example 5
The embodiment provides a preparation method of nontoxic tissue slice mounting glue, which comprises the following steps: and fully mixing 85 parts by weight of isooctyl polymethacrylate mixed glue, 5 parts by weight of limonene and 10 parts by weight of fir glue at normal temperature to obtain the mounting glue.
The mixed glue of the isooctyl methacrylate is prepared by 60 weight parts of isooctyl methacrylate, 40 weight parts of D30 solvent oil and 1.38 weight parts of guiding agent (benzoyl peroxide), and the specific preparation method of the mixed sol of the isooctyl methacrylate is as follows:
(1) initial polymerization reaction: fully and uniformly mixing 60 parts by weight of isooctyl methacrylate and 40 parts by weight of D30 solvent oil at normal temperature, adding the mixture into a reaction kettle, controlling the temperature to be 110-120 ℃, continuously stirring at the stirring speed of 120r/min, then adding 0.1 part by weight of guiding agent every 10min, controlling the total addition of the guiding agent to be 0.3 part by weight, and carrying out primary polymerization for 30 min;
(2) and (3) repolymerization: and continuously heating the primary polymerization reaction product to 140-145 ℃, preserving heat, continuously stirring at the stirring speed of 120r/min, adding 0.18 part by weight of the guiding agent every 20min for 6 times, preserving heat and reacting for 40min, and finishing the polymerization reaction.
Example 6
This example differs from example 1 in that: the directing agent was azobisisobutyronitrile, the rest being carried out as in example 1.
Example 7
This example differs from example 2 in that: the directing agent was azobisisobutyronitrile, the rest being carried out as in example 2.
Example 8
This example differs from example 5 in that: the directing agent was azobisisobutyronitrile, the rest being carried out as in example 5.
The beneficial effects that can be obtained by the present invention are illustrated by the following experiments:
the following criteria were determined for the non-toxic tissue slice mounting adhesives prepared according to the methods of examples 1-8 and compared with the quality parameters of commercially available neutral and fir glues, and the results are shown in table 1.
TABLE 1 average parameter comparison results of mounting adhesives prepared in examples 1-8 of the present invention with neutral and fir glues
Those skilled in the art know that: the quick-drying speed of the sealing glue is high, the refractive index is excellent between 1.52 and 1.53, the viscosity is excellent between 150 and 160mPa.s, the cost is low, and no toxicity is high.
As can be seen from the data in table 1: by comparing examples 1-8 of the present invention with neutral and fir gums, it can be seen that: compared with the existing fir glue and neutral glue, the sealing glue prepared by the embodiment of the invention has the characteristics of high drying speed, good refractive index, high viscosity, low cost, no toxicity and environmental friendliness. By comparing examples 1 to 8 of the present invention: the effects of example 2, example 3, and example 7 are superior to those of example 1 and example 4, example 5, example 6, and example 8, and the effect of example 7 is superior to those of examples 6 and 8, in which: the mounting adhesive prepared according to the embodiment 2 and the embodiment 7 has the best effect in all aspects, so the embodiment is the best embodiment; the preferred formula of the mounting adhesive of the invention is as follows: 85-96 parts by weight of isooctyl methacrylate mixed sol, 2-5 parts by weight of limonene and 2-10 parts by weight of fir glue, wherein the isooctyl methacrylate mixed sol is prepared from 50-60 parts by weight of isooctyl methacrylate, 40-50 parts by weight of D30 solvent oil and 0.9-1.5 parts by weight of guiding agent (benzoyl peroxide or azobisisobutyronitrile); the formula is further preferably 90-93 parts by weight of isooctyl methacrylate mixed glue, 3-4 parts by weight of limonene and 4-6 parts by weight of fir glue, wherein the isooctyl methacrylate mixed glue is prepared by 54-58 parts by weight of isooctyl methacrylate, 42-46 parts by weight of D30 solvent oil and 1.14-1.38 parts by weight of guiding agent (benzoyl peroxide or azobisisobutyronitrile).
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (4)
1. A preparation method of nontoxic tissue slice mounting glue is characterized in that 92 parts by weight of isooctyl polymethacrylate mixed glue, 3 parts by weight of limonene and 5 parts by weight of fir glue are mixed to obtain the mounting glue; the isooctyl methacrylate mixed glue is prepared from 55 parts by weight of isooctyl methacrylate, 45 parts by weight of D30 solvent oil and 1.2 parts by weight of guiding agent.
2. The method for preparing a nontoxic tissue slice mounting gel according to claim 1, wherein the guiding agent is benzoyl peroxide or azobisisobutyronitrile.
3. The method for preparing non-toxic tissue slice mounting adhesive according to claim 1, wherein the method for preparing the mixed glue of isooctyl methacrylate comprises the following steps:
1) initial polymerization reaction: fully and uniformly mixing isooctyl methacrylate and D30 solvent oil by 100 parts by weight, adding the mixture into a reaction kettle, continuously stirring, controlling the stirring speed of a stirring paddle to be 120r/min, controlling the temperature to be 110-120 ℃, then adding 0.1 part by weight of guiding agent every 10min, controlling the total adding amount of the guiding agent to be 0.3 part by weight, and carrying out primary polymerization for 30 min;
2) and (3) repolymerization: and continuously heating the primary polymerization reactant to 140-145 ℃, preserving the heat, continuously stirring, adding 0.1-0.2 part by weight of the guiding agent into the mixture every 20min at the stirring speed of 120r/min for 6 times, preserving the heat and reacting for 40min, and finishing the polymerization reaction.
4. The method for preparing non-toxic tissue slice mounting adhesive according to claim 3, wherein the guiding agent in the step 2) is added in an amount of: 0.14 to 0.18 parts by weight of the additive is added every 20min for 6 times in total.
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| AU3744299A (en) * | 1998-04-09 | 1999-11-01 | 3M Innovative Properties Company | Adhesive cover slip and method for microscopy |
| BRPI0617836A2 (en) * | 2005-10-26 | 2011-08-09 | Lee H Angros | microscope slide cover plate, microscope slide cover plate set, and method of forming a microscope slide cover plate set |
| KR101811073B1 (en) * | 2010-01-29 | 2017-12-20 | 다이니폰 인사츠 가부시키가이샤 | Microorganism culture sheet |
| CN106370503A (en) * | 2016-08-31 | 2017-02-01 | 宁波同盛生物科技有限公司 | Organic quick drying mounting medium |
| CN107488424B (en) * | 2017-08-25 | 2019-05-21 | 宁波同盛生物科技有限公司 | A kind of no benzene mountant and preparation method thereof |
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