Firing method of low-temperature fast-firing glazed tile and low-temperature fast-firing glazed tile
阅读说明：本技术 低温快烧釉面砖的烧成方法及低温快烧釉面砖 (Firing method of low-temperature fast-firing glazed tile and low-temperature fast-firing glazed tile ) 是由 母军 梁广波 赖振煌 魏麟凯 姜文炜 金杰 于 2020-04-27 设计创作，主要内容包括：本发明公开了一种低温快烧釉面砖的烧成方法,其包括：(1)将各种原料混合均匀,然后经球磨制浆、喷雾制粉、压制、干燥、施釉后得到生坯；(2)将所述生坯按照预设烧成曲线烧成,即得到低温快烧釉面砖成品；其中,预设烧成曲线包括先升温至1150℃,然后降温至900～1100℃,再升温至烧成温度,保温预设时间后降温至80～300℃。相应的,本发明还公开了一种低温快烧釉面砖,其采用上述烧成方法烧制而得。本发明采用先升温、后降温、再升温、保温、降温的烧成方法,使得主矿相-莫来石的生长时间变长；从而提升了产品强度,缩短了烧成时间。同时,本发明的烧成方法还可有效降低返变现象发生的概率。(The invention discloses a firing method of a low-temperature fast-fired glazed tile, which comprises the following steps: (1) uniformly mixing various raw materials, and then performing ball milling pulping, spray milling, pressing, drying and glazing to obtain a green body; (2) firing the green body according to a preset firing curve to obtain a finished product of the low-temperature fast-fired glazed tile; wherein the preset firing curve comprises the steps of firstly heating to 1150 ℃, then cooling to 900-1100 ℃, then heating to the firing temperature, preserving heat for a preset time, and then cooling to 80-300 ℃. Correspondingly, the invention also discloses a low-temperature fast-fired glazed tile which is fired by adopting the firing method. The invention adopts a sintering method of firstly heating, then cooling, then heating, heat preservation and cooling, so that the growth time of the main mineral phase-mullite is prolonged; thereby improving the strength of the product and shortening the sintering time. Meanwhile, the sintering method of the invention can also effectively reduce the probability of occurrence of the return phenomenon.)
1. A firing method of a low-temperature fast-fired glazed tile is characterized by comprising the following steps:
(1) uniformly mixing various raw materials, and then performing ball milling pulping, spray milling, pressing, drying and glazing to obtain a green body;
(2) firing the green body according to a preset firing curve to obtain a finished product of the low-temperature fast-fired glazed tile;
wherein the preset firing curve is as follows:
heating the mixture from room temperature to 1150 ℃, wherein the heating rate is 160-200 ℃/min;
cooling from 1150 ℃ to T1The cooling rate is 6-10 ℃/min;
from T1Heating to the firing temperature, wherein the heating rate is 40-80 ℃/min;
keeping the temperature at the firing temperature for 5-15 min;
cooling from sintering temperature to T2The cooling rate is 90-150 ℃/min;
wherein, T is1900-1100 ℃, the firing temperature is 1150-1170 ℃, and T2Is 80 to 300 ℃.
2. The firing method of a low-temperature fast-fired glazed tile according to claim 1, wherein the preset firing curve is:
heating the mixture from room temperature to 1150 ℃, wherein the heating rate is 160-180 ℃/min;
cooling from 1150 ℃ to T1The cooling rate is 8-10 ℃/min;
from T1Heating to a sintering temperature, wherein the heating rate is 50-70 ℃/min;
keeping the temperature at the firing temperature for 8-12 min;
cooling from sintering temperature to T2The cooling rate is 100-130 ℃/min;
wherein, T is11000-1100 ℃, the firing temperature is 1160-1170 ℃, and T2Is 100 to 250 ℃.
3. The firing method of a low-temperature fast-fired glazed tile as claimed in claim 1, wherein in the step (1), the raw materials are uniformly mixed according to the formula; the formula mainly comprises the following raw materials in parts by weight:
8-12 parts of sodalite powder, 35-42 parts of potassium-sodalite powder, 2-5 parts of high-temperature sand, 10-15 parts of medium-temperature sand, 0.1-5 parts of additive, 3-8 parts of black mud, 7-12 parts of kaolin, 12-17 parts of washing mud and 2-4 parts of talc; the sum of the weight parts of the raw materials is 100 parts.
4. The firing method of the low-temperature fast-firing glazed tile as claimed in claim 3, wherein the formulation mainly comprises the following raw materials in parts by weight:
9-10 parts of sodalite powder, 36-40 parts of potassium-sodalite powder, 3-5 parts of high-temperature sand, 13-15 parts of medium-temperature sand, 2-5 parts of additives, 4-6 parts of black mud, 8-10 parts of kaolin, 12-15 parts of washing mud and 2.5-4 parts of talc; the sum of the weight parts of the raw materials is 100 parts.
5. The firing method of a low-temperature fast-firing glazed tile according to claim 3, wherein the formulation further comprises 0.1 to 1 part of a reinforcing agent and 0.1 to 1 part of a debonding agent.
6. The firing method of the low-temperature fast-firing glazed tile according to claim 3, wherein the additive comprises the following chemical components in percentage by weight:
SiO273～76％，Al2O317～20％，Fe2O30.05～0.15％，TiO20.1～0.2％，CaO 0.1～0.2％，MgO 0.1～0.2％，K2O 1.5～2.0％，Na2O 0.3～0.5％，LOI 3.5～4.0％。
7. the firing method of the low-temperature fast-firing glazed tile according to claim 6, wherein the additive comprises the following chemical components in percentage by weight:
SiO274～76％，Al2O318～20％，Fe2O30.05～0.1％，TiO20.1～0.2％，CaO 0.1～0.2％，MgO 0.1～0.2％，K2O 1.8～2.0％，Na2O 0.3～0.5％，LOI 3.5～4.0％。
8. the method of claim 1, wherein Al is present in the green body2O3The content is 15-18 wt%, and the loss on ignition is 2-4 wt%.
9. The method for firing a glazed tile at a low temperature and in a rapid firing manner as claimed in claim 5, wherein the dispergator is sodium tripolyphosphate and the reinforcing agent is PVA.
10. A low-temperature fast-fired glazed tile, which is obtained by firing the low-temperature fast-fired glazed tile according to any one of claims 1 to 9.
Technical Field
The invention relates to the technical field of ceramic tiles, in particular to a low-temperature fast-fired glazed tile and a firing method thereof.
Background
On one hand, in the existing ceramic tile firing field, a gradient firing curve, namely a process of gradually raising temperature, preserving heat and gradually lowering temperature, is adopted; this process is time consuming.
On the other hand, in the production process of traditional porcelain glazed tiles, such as archaized tiles, full-glazed tiles and the like, in order to ensure that products are not deformed and have high strength (modulus of rupture) and certain qualification rate, Al in a blank body is always required to be removed2O3The content is controlled to be 19-22%. In the finished low-temperature quick-fired glazed tile, Al2O3In the form of mullite and glass phase; wherein, the mullite phase can improve the strength; and maintaining the balance of the glass phase and the mullite phase can effectively eliminate stress and control the deformation of the fired ceramic tile.
In conventional ceramic raw materials, Al2O3The sources of (A) are in three categories: the first kind is clay raw material, such as kaolin, bentonite, black mud, white mud, washing soil and the like; the second kind is flux raw materials, such as potassium feldspar, albite and various sand materials; the third type is some high-alumina type raw materials, such as bauxite, mullite, alumina and the like. In order to maintain Al in the low-temperature fast-fired glazed tile blank2O3The content is between 19 and 22 percent, bauxite needs to be added or a large amount of clay raw materials (accounting for 25 to 40 percent) needs to be adopted; however, bauxite can greatly increase the sintering temperature and prolong the sintering time; in addition, because of gradual exhaustion of high-quality kaolin raw material in ChinaAnd the ecological environmental protection policy is gradually implemented, and high-quality raw materials with high alumina content, such as kaolin black mud, are increasingly scarce. The clay raw material is supplied in a smaller and smaller amount under the background of national environmental protection policy. Therefore, there is an urgent need to consider the reduction of Al in low-temperature fast-fired glazed tiles2O3And (4) content.
However, when Al is reduced2O3After the content is increased, the mullite content in the green body is correspondingly reduced, so that the stress accumulation in the firing process is large, and the deformation is easy to occur; particularly, after the firing was left for 15 days, the ceramic composition was very likely to be deformed (reversion). At the same time, Al is reduced2O3After the content, the strength of the fired product is reduced; in addition, the blank glaze adaptability is reduced, and edge crack is caused.
Disclosure of Invention
The invention aims to solve the technical problem of providing a firing method of a low-temperature fast-fired glazed tile, which has short firing period and low firing energy consumption.
The technical problem to be solved by the invention is to provide a low-temperature fast-fired glazed tile which has high strength and small deformation.
In order to solve the above problems, the present invention provides a firing method of a low-temperature fast-fired glazed tile, comprising:
(1) uniformly mixing various raw materials, and then performing ball milling pulping, spray milling, pressing, drying and glazing to obtain a green body;
(2) firing the green body according to a preset firing curve to obtain a finished product of the low-temperature fast-fired glazed tile;
wherein the preset firing curve is as follows:
heating the mixture from room temperature to 1150 ℃, wherein the heating rate is 160-200 ℃/min;
cooling from 1150 ℃ to T1The cooling rate is 6-10 ℃/min;
from T1Heating to the firing temperature, wherein the heating rate is 40-80 ℃/min;
keeping the temperature at the firing temperature for 5-15 min;
cooling from sintering temperature to T2The cooling rate is 90-150 ℃/min;
wherein, T is1900-1100 ℃, the firing temperature is 1150-1170 ℃, and T2Is 80 to 300 ℃.
As an improvement of the above technical solution, the preset firing curve is:
heating the mixture from room temperature to 1150 ℃, wherein the heating rate is 160-180 ℃/min;
cooling from 1150 ℃ to T1The cooling rate is 8-10 ℃/min;
from T1Heating to a sintering temperature, wherein the heating rate is 50-70 ℃/min;
keeping the temperature at the firing temperature for 8-12 min;
cooling from sintering temperature to T2The cooling rate is 100-130 ℃/min;
wherein, T is11000-1100 ℃, the firing temperature is 1160-1170 ℃, and T2Is 100 to 250 ℃.
As an improvement of the technical scheme, in the step (1), various raw materials are uniformly mixed according to a formula; the formula mainly comprises the following raw materials in parts by weight:
8-12 parts of sodalite powder, 35-42 parts of potassium-sodalite powder, 2-5 parts of high-temperature sand, 10-15 parts of medium-temperature sand, 0.1-5 parts of additive, 3-8 parts of black mud, 7-12 parts of kaolin, 12-17 parts of washing mud and 2-4 parts of talc; the sum of the weight parts of the raw materials is 100 parts.
As an improvement of the technical scheme, the formula mainly comprises the following raw materials in parts by weight:
9-10 parts of sodalite powder, 36-40 parts of potassium-sodalite powder, 3-5 parts of high-temperature sand, 13-15 parts of medium-temperature sand, 2-5 parts of additives, 4-6 parts of black mud, 8-10 parts of kaolin, 12-15 parts of washing mud and 2.5-4 parts of talc; the sum of the weight parts of the raw materials is 100 parts.
As an improvement of the technical scheme, the formula further comprises 0.1-1 part of a reinforcing agent and 0.1-1 part of a debonding agent.
As an improvement of the technical scheme, the additive comprises the following chemical components in percentage by weight:
SiO273～76％，Al2O317～20％，Fe2O30.05～0.15％，TiO20.1～0.2％，CaO 0.1～0.2％，MgO 0.1～0.2％，K2O 1.5～2.0％，Na2O 0.3～0.5％，LOI 3.5～4.0％。
as an improvement of the technical scheme, the additive comprises the following chemical components in percentage by weight:
SiO274～76％，Al2O318～20％，Fe2O30.05～0.1％，TiO20.1～0.2％，CaO 0.1～0.2％，MgO 0.1～0.2％，K2O 1.8～2.0％，Na2O 0.3～0.5％，LOI 3.5～4.0％。
as an improvement of the technical proposal, Al in the green body2O3The content is 15-18 wt%, and the loss on ignition is 2-4 wt%.
As an improvement of the technical scheme, the dispergator is sodium tripolyphosphate, and the reinforcing agent is PVA.
Correspondingly, the invention also discloses a low-temperature fast-fired glazed tile, which is fired by adopting the firing method of the low-temperature fast-fired glazed tile.
The implementation of the invention has the following beneficial effects:
1. the invention adopts a sintering method of firstly heating, then cooling, then heating, heat preservation and cooling, so that the growth time of the main mineral phase-mullite is prolonged; thereby improving the strength of the product and shortening the sintering time. In the invention, the firing period is 30-40 minutes, and the firing period of the conventional low-temperature quick-fired glazed tile is 50-80 minutes.
2. According to the invention, a high amount of talc is introduced into the formula, and a traditional Na-K-Al-Si system phase diagram is converted into a Na-K-Al-Si-Mg system phase diagram; simultaneously, the invention also introduces an additive, the additive and the sintering curve can be effectively matched, the precipitation of mullite phase is promoted, the heat stress accumulation in the sintering process is reduced, and the problem of Al2O3The strength is reduced and the reversion is increased due to the reduction of the content.
3. In the formula, the content of the scarce mud raw materials (black mud and washing mud) is 10-20 parts; is lower than 25-40% of the existing low-temperature quick-fired glazed tile; the raw material cost is reduced.
4. In the formula, the loss on ignition is 3.5-4%, and the method is suitable for quick firing, greatly shortens the firing period and improves the yield. The overall firing period of the low-aluminum high-silicon high-strength non-deformation glazed tile is 30-40 min. In addition, the aluminum oxide content is low, the method is suitable for low-temperature sintering, and the sintering energy consumption is reduced. Specifically, the sintering temperature in the invention is reduced from 1225 ℃ to 1150-1170 ℃ in the prior art, and the sintering energy consumption is saved by 10-20%. Specifically, the sintering temperature in the invention is reduced from 1225 ℃ to 1150-1170 ℃ in the prior art, and the sintering energy consumption is saved by 10-20%.
Drawings
FIG. 1 is a flow chart of a firing method for a low-temperature fast-firing glazed tile of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below.
Referring to fig. 1, the present invention provides a firing method of a low-temperature fast-fired glazed tile, comprising the steps of:
s1: uniformly mixing various raw materials, and then performing ball milling pulping, spray milling, pressing, drying and glazing to obtain a green body;
s2: firing the green body according to a preset firing curve to obtain a finished product of the low-temperature fast-fired glazed tile;
wherein the preset firing curve is as follows:
heating the mixture from room temperature to 1150 ℃, wherein the heating rate is 160-200 ℃/min;
cooling from 1150 ℃ to T1The cooling rate is 6-10 ℃/min;
from T1Heating to the firing temperature, wherein the heating rate is 40-80 ℃/min;
keeping the temperature at the firing temperature for 5-15 min;
cooling from sintering temperature to T2The cooling rate is 90-150 ℃/min;
wherein, T is1900-1100 ℃, the firing temperature is 1150-1170 ℃, and T2Is 80 to 300 ℃.
Based on the sintering method of the embodiment, the sintering method of firstly heating, then cooling, then heating, preserving heat and finally cooling is adopted, so that the retention time of the green body within 900-1150 ℃ can be effectively prolonged, and mullite grains are fully precipitated. Particularly, a temperature reduction method is adopted within 1150-900 ℃, so that the size of mullite grains is effectively controlled and is relatively small. And then effectively promoted intensity, reduced thermal stress accumulation, reduced later stage rate of return.
In addition, when the sintering method is adopted, the heating rate and the cooling rate can be effectively improved, so that the whole sintering period is shortened; in the invention, the firing period is 30-40 minutes; the firing period of the ordinary low-temperature quick-firing glazed tile needs 50-80 minutes.
In an alternative embodiment, the step S1 includes:
s11: uniformly mixing various raw materials according to a formula to obtain a mixture;
s12: ball milling and pulping the mixture, and spraying and pulverizing to obtain powder;
in an alternative embodiment, the formula in S11 mainly comprises the following raw materials in parts by weight:
9-10 parts of sodalite powder, 36-40 parts of potassium-sodalite powder, 3-5 parts of high-temperature sand, 13-15 parts of medium-temperature sand, 2-5 parts of additives, 4-6 parts of black mud, 8-10 parts of kaolin, 12-15 parts of washing mud and 2.5-4 parts of talc; the sum of the weight parts of the raw materials is 100 parts.
Based on the formula, Al in the green body2O315-19 wt%, 2.5-4% of MgO and 3-4% of loss on ignition. On one hand, the traditional Na-K-Al-Si system phase diagram is converted into a Na-K-Al-Si-Mg system phase diagram, the components of the high-temperature solid solution are changed, so that the alumina in the blank is quickly dissolved into the high-temperature solid solution, and therefore, on the contact surface of the alumina and the molten solution, free silica is combined with the alumina to react to form mullite, and the precipitation of the mullite is promoted; furthermore, this is achievedThe mullite formed by the seed reaction is mostly secondary mullite, and the length of the mullite column is longer, thereby solving the problem of Al2O3The strength is reduced, the deformation is increased, and the reversion is increased due to the reduction of the content, so that the qualification rate is improved. On the other hand, the above-mentioned transformation of the phase diagram allows the formulation to be well matched with the firing curve.
In addition, after the phase diagram system is converted, the expansion coefficient of the blank is also changed in a large range; therefore, the invention also introduces an additive which can be combined with the talc and other raw materials to adjust the expansion coefficient of the green body, reduce the stress accumulation in the firing process and prevent the reversion. In addition, the additive can also act synergistically with the talc to promote the precipitation of secondary mullite in a Na-K-Al-Si phase diagram.
Furthermore, in the formula, the content of mud raw materials (washed mud and black mud) is low, and the raw material cost of the low-temperature quick-fired glazed tile is reduced.
Specifically, in the above formula, the main mineral phase of the albite powder is albite, and a small amount of quartz, potassium feldspar, plagioclase feldspar and the like are often doped (it is difficult to find pure mineral in nature). In the soda stone powder of the present invention, Na is contained2The content of O is 6-10 wt%. In the formula of the invention, the dosage of the sodium stone powder is 8-12 parts, and can be 8 parts, 9 parts, 10 parts, 11 parts and 12 parts by way of example; preferably, the using amount of the sodium stone powder is 9-10 parts.
Specifically, in the above formula, the main mineral phases of the potassium-sodium stone powder are microcline feldspar and potassium feldspar, and some mineral phases such as quartz, albite and the like are often doped. In the potassium-sodium stone powder of the invention, K24 to 10 wt% of O, and Na2The content of O is 2-5 wt%. In the formula of the invention, the dosage of the potassium-sodium stone powder is 35-42 parts, and can be 35 parts, 36 parts, 38 parts, 11 parts and 12 parts by way of example; preferably, the using amount of the potassium-sodium stone powder is 36-40 parts.
The main mineral phases of the high-temperature sand are quartz, kaolinite and mica, and some potassium feldspar, albite, plagioclase feldspar and the like can be doped. The mullite fiber mainly plays a role of aggregate, and a small amount of mullite can be separated out, so that the strength is improved. In the present invention, Al is contained in the high-temperature sand2O3The content is 19-22％，K2O and Na2The sum of the contents of O is 0.1-3 wt%, and the high-temperature sand in the range can provide alumina and free silica when being fired, wherein the alumina can be dissolved in molten liquid, so that the free silica and the alumina dissolved in the molten liquid react to form secondary mullite.
The main mineral phase of the medium-temperature sand is basically the same as that of the high-temperature sand, but the contents of all the mineral phases are different, so that the chemical components of the medium-temperature sand are different from those of the high-temperature sand; al in medium-temperature sand2O317 to 20 wt.%, K2O and Na2The sum of the O content is 2-6 wt%; the method plays a more role in adjusting a high-temperature molten phase in the sintering process, and can also separate out a small amount of mullite.
Black mud is a major clay-based mineral, and more particularly, it belongs to ball clay-based clay; the main mineral phases of the mineral are kaolin, quartz, mica and some organic matters. According to the invention, the content of black mud is reduced to 3-8 parts, and the raw material cost is effectively reduced.
The washed mud is another main clay mineral, and is prepared by removing sand and organic matters from raw ore mud (black mud, white mud and the like) and then performing filter pressing. Washing mud is one of the main mullite sources.
Kaolin is also a major clay mineral, which is usually associated with quartz, mica, in nature. Kaolin being Al2O3One of mullite sources. Specifically, in the present invention, Al is contained in kaolin2O3The content is 25 to 35 wt%.
Specifically, in the formula of the low-temperature fast-fired glazed tile, the content of the talc is 2.5-4 parts; in the traditional formula, the content of the talc is generally below 1.5 percent, the talc content is increased, the phase diagram in the invention can be converted from the traditional Na-K-Al-Si system phase diagram into the Na-K-Al-Si-Mg system phase diagram, the components of the high-temperature solid solution are changed, the alumina in the blank is rapidly dissolved into the high-temperature solid solution, and therefore, on the contact surface of the alumina and the molten liquid, free silica is combined with the alumina to react to form mullite, and the precipitation of the mullite is promoted; in addition, mullite is formed by this reactionThe majority of stones are secondary mullite with longer mullite column length, thereby solving the problem of Al2O3The strength is reduced, the deformation is increased, and the reversion is increased due to the reduction of the content, so that the qualification rate is improved. Meanwhile, the talc can effectively adjust high-temperature molten phase components and reduce stress accumulation.
In addition, the formula of the invention also introduces an additive, and the chemical component of the additive is SiO273～76％，Al2O317～20％，Fe2O30.05～0.15％，TiO20.1～0.2％，CaO 0.1～0.2％，MgO 0.1～0.2％，K2O1.5～2.0％，Na20.3-0.5% of O and 3.5-4.0% of LOI. The additive can act together with the formula and the firing curve, improve the expansion coefficient of the green body, improve the adaptability of the green body and the glaze, reduce the stress accumulation in the firing process and effectively prevent the reversion. In addition, the additive of the present invention can replace common high aluminum materials. Preferably, the chemical components of the additive are as follows: SiO 2274～76％，Al2O318～20％，Fe2O30.05～0.1％，TiO20.1～0.2％，CaO 0.1～0.2％，MgO 0.1～0.2％，K2O 1.8～2.0％，Na2O 0.3～0.5％，LOI 3.5～4.0％。
In addition, the invention reduces Al by reducing the content of mud raw materials (washed mud and black mud)2O3The purpose of content. In order to solve the problem of strength reduction of mud raw materials, 0.1-1 part of a reinforcing agent and 0.1-1 part of a debonding agent are added into the formula, so that the strength of the mud raw materials can be improved, and drying cracking can be prevented. Specifically, the dispergator is sodium tripolyphosphate, and the reinforcing agent is PVA.
S13: distributing the powder for the second time, pressing, drying and glazing to obtain a green body;
the invention changes the traditional primary cloth into the secondary cloth and changes the traditional single-layer green body structure into the double-layer green body structure, thereby being very beneficial to the discharge of volatile matters and improving the structure in the aspect of later improvement.
In an alternative embodiment, the firing profile in step S2 is:
(1) heating the mixture from room temperature to 1150 ℃, wherein the heating rate is 160-200 ℃/min;
the Loss On Ignition (LOI) of the formula of the invention is less than 4 percent, so that the invention can adopt a high temperature rise rate in the prior oxidation stage. Specifically, the heating rate is 160, 170, 185, 190, 200 ℃/min; preferably, the heating rate is 160-180 ℃/min;
(2) cooling from 1150 ℃ to T1The cooling rate is 6-10 ℃/min;
in particular, T1900 to 1100 ℃, preferably 1000 to 1100 ℃. The temperature reduction operation is adopted in the temperature range, so that the retention time in the range of 900-1150 ℃ can be prolonged, and the content of the mullite phase is improved.
Specifically, the cooling rate is 6-10 ℃/min; specifically, the cooling rate can be 6, 7, 8, 9, 10 ℃/min; the preferable rate is 8-10 ℃/min; the cooling is carried out at the cooling rate, so that the refining of mullite grains can be promoted, and the mullite grains with smaller grain size are more favorable for promoting the strength to be improved, reducing the heat stress accumulation and reducing the reversion.
(3) From T1Heating to the firing temperature, wherein the heating rate is 40-80 ℃/min;
specifically, the firing temperature is 1150-1170 ℃; preferably 1160-1170 ℃; the formula of the low-temperature fast-firing glazed tile is lower in firing temperature and saves energy.
Specifically, the heating rate can be 40, 45, 55, 60, 75, 80 ℃/min; preferably, the heating rate is 50-70 ℃/min.
(4) Keeping the temperature at the firing temperature for 5-15 min;
(5) cooling from sintering temperature to T2The cooling rate is 90-150 ℃/min;
wherein, T2Is 80 to 300 ℃. Preferably 100 to 250 ℃.
The present invention will be described with reference to specific examples.
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