JPS58154798A - Heat dehydration of brown coal - Google Patents

Abstract

PURPOSE:To stabilize operation in a hydroliquefaction step by converting Ca, etc. in coal into a minute carbonate particle by injecting CO2-contg. gas produced in a gas/liquid separator into raw slurry in a heating to gas/liquid separation step. CONSTITUTION:Slurry S consisting of raw brown coal and a solvent (numeral 1 represents a ball mill, and 2 a slurry tank) is pressurized by a pump 3, sent with addition of a CO2-contg. gas to a heat exchanger 4, in which the water content is reduced to about 10%, and introduced into a gas/water separator 5 after Ca, etc. in the coal is converted into a minute carbonate particle and stabilized. Then the separated liquid phase portion (contg. calcium carbonate, etc.) is sent to a hydrogenation step, while the separated gas phase portion (contg. steam, CO2, etc.) is sent to a CO2 separator, and the separated CO2-contg. gas is supplied to a heat exchanger 4 and the gas/water separator 5, wherein, if necessary, CO2 is further added from outside the system.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention is based on an improvement of the brown #IO extraction water tying method and the pretreatment method. The present invention relates to a method for removing moisture and preventing the formation of sediment and scale in a reaction system.

As a method for liquefying coal, there is known a method in which coal is mixed with fIIIAIIIl to sludge and only the O#I agent extract in the coal is subjected to water S liquefaction, that is, the extraction water temperature liquefaction method.

However, Hashi O stone IN has a high water content, and in particular, the water content of Hashi O stone IN can be as high as Fi@O*, so it is uneconomical from a thermal efficiency point of view to subject it to the 1-heavy liquefaction treatment. It is. Therefore, when using such coking coal, it is necessary to dehydrate it before supplying it to the liquefaction process.
When the conventional #i flash drying method is applied, the moisture content is reduced to 1 by
It was lowered to around 0. However, this method has the drawbacks of requiring enormous enthusiasm for airflow heating, the formation of purulence on the brown leg grains, and inhibiting the progress of the hydrogenation and liquefaction reaction. Since it has the disadvantage that the volatile components in the coal decompose and reduce the liquefaction yield, it is difficult to use in practical use.For this reason, the applicant has decided to heat the coking coal A steam heat exchange method in which moisture in coking coal is separated as steam and this high-temperature fli9K is used for heating the raw material *0 was previously published in Patent J13 (Japanese Patent Laid-Open No. 11fi8-112902). The key point of the method is to mix raw lignite with a solvent to form a slurry, pass it through a heat exchanger to preheat it, and then
GCFII separation is carried out by heating to 800°C, and while the dehydrated slurry is collected, the separated water vapor is
The pre-JlO defect was resolved at once by the presence of O'chl and keratin at the point where it was circulated through the heat exchanger and used as a preheating source for the raw material 91-.

By this method, the moisture content in lignite can be removed in a very efficient manner and legally, but brown coal
) vh is now open, but Ilm is a problem that can be solved in parallel. In other words, X whose main raw material is lignite
If 9$- is applied to the extraction-based liquefaction method, the preheater and
Continuous operation at 18% A with a large amount of material deposited in the slurry transport piping, resulting in a serious scaling accident and causing great damage. There is. So I went to Shenbong-Nakasuka.
When it became necessary to purchase a new solution, I researched these OX- and was convinced that metallic coal #wood was playing an important role.
It is reported that 44% by weight of the ash contained in the ash was impregnated with wood-forming metal components (hereinafter typically referred to as C & etc.). There is also. Moreover, brown lII has stone structure characteristics such as water #ink, mA/BOKIFA/group, carbonyl group, etc.
Contains Ill-containing substituents, these substituents are easily decomposed in the water conversion reaction step during the stone dissolution step,
There is a background that KHgO, COQ, Co, etc. are generated within the system. These Richi HIO#i directly amplify the problem of increased water content, lower the water volume partial pressure in the reaction process and lower the liquid efficiency, and COg and CO react with the Ca coexisting in the system. The acid builds up and causes scale formation in the sediment.

In other words, considering the special circumstances (excessive water content and formation of oil such as sediment) when lignite is hydrogenated and liquefied, the two major defects mentioned above are solved simultaneously, but in the water #i liquefaction treatment of lignite, We have reached the conclusion that it is very advantageous from an economic point of view.6 The present invention was made in consideration of this situation, and
It shows sufficient dehydration effect in the first stage of preliminary treatment, and removes Ca etc. on the first floor as possible! Chemotaxis and hydrogenation liquefaction stage K
The constraint is to establish a method that can conveniently achieve the two-person goal of preventing the formation of JP-ketsu-kyou-ki.

The main point of the method of the present invention is to achieve the above objectives by elevating the raw material consisting of raw brown coal and a solvent.
Gas-liquid decomposition under external pressure and release of water with a steam wand, a airlessness is sura V-o! In addition to using it as a heat source for iF warming,
*'x The 0g-containing gas and/or the COQ-containing gas that is supplied during the liquid separation process is injected into the raw material slurry in the elevating process or the gas-liquid separation process. This is to actively stabilize C. Lu-hyun as a single-minded ms woodcutter at this stage. In other words, the removal of wood and #11 salt precipitation stabilization process are performed in parallel as a pretreatment site for hydrogenation and liquefaction. The above point has all been resolved. In other words, although the economical dehydration effect has already been mentioned, the 1
11111 The woodcutter is sent to the water temperature liquefaction process without being separated as it is, and it does not dissolve again in the anti-MS liquid, so SRC#ll1
It does not have an adverse effect on the KL process, and since it is extremely fine-grained and highly buoyant, it does not precipitate on the catalyst or vessel wall, and there is no risk of single-grain growth leading to deposition or scale formation. Therefore, no scaling accident occurred during the closing accident, and continuous operation under stable conditions became possible.

Next, the structure and effects of the present invention will be clarified based on diagrams showing examples.

FIG. 1 shows a 00g-containing gas (
Although it includes CO gas, etc., it is expressed as a single KCOg in the drawings and specification) and /* is a flow diagram showing an example in which CO2 supplied from outside the i system is injected. That is, raw brown leg, a low boiling point solvent and a high boiling point solvent are used as raw materials, and after receiving catalyst particles added as necessary in a ball mill 1 installed according to the IK, it is introduced into a slurry tank 2. After sufficient mixing, the raw material 91j- (hereinafter referred to as suri IIi in Kg) is obtained. Regarding the total amount of the # agent in the tie, there is no particular rule, as Arihashi*i, which has an appropriate viscosity throughout the entire process, is used.

Slurry S is pressurized by pump 8 and sent to heat exchanger 4.
The water in the slurry s is evaporated by heating with a trowel, but if necessary, the slurry is then introduced into a suitable heating device to further evaporate the water sufficiently and reduce the water content to the target water content (approximately below the tall). The ceramic heating layer N is sent to the gas-liquid separator 5 at a temperature of 100 to 400° C., preferably 110 to 860° C., under pressure such that moisture is sufficiently evaporated at a room temperature. granite heat exchange 814
The heat source is steam sent from the pressurizing means described below, and the steam is subjected to heat exchange, then cooled, and immersed in oil and moisture awe to recover the low cotton spot l# agent. It will be done. 9L14! Slurry sF supplied to separation J[
i, the above steam I! (hereinafter referred to as steam), as well as
Reactions with Ca, etc. are progressing in response to the cogo supply sent from the outside of the thread or from the removed CogM11, so each JllII
Contains fine grains of Kizuna O and unreacted gas phase C02. Therefore, in electrolyte separation-6, steam and gt-phase COg gas are separated from the slurry and the production leg wood, and this separated gas is sent to the COg removal device B. In the case of decolonization, for example, CO2 is removed by a CO2 adsorption method or a steam condensation and reheating method.
Separation of O2 gas and steam is performed, and each is confirmed as described above, but if non-condensable gases such as CO2 and CO are included in the circulating steam, heat exchange is required! 11 The heat transfer effect within the vessel 4 is poor, and the thermal efficiency decreases, so COa and c
o should be removed as much as possible (it is recommended.
It is recommended that the steam purified by ommm is pressurized by the booster 0 and the pressurizing means 8, and that it is heated in accordance with the aI pressure increase before being sent to the heat exchanger #1. On the other hand, the slurry exchanger coming out of the gas-liquid separation 6 is combined with some f# agent recovered from the COga removal 6, and then sent to the primary hydrogenation step 7 to undergo a hydrogenation and liquefaction reaction. It costs ¥11 to recover and recycle from the high boiling point tank used for mixing with the probiotic brown leg in the primary hydrogenation step 7.

In this embodiment, COg inside the system or COg outside the system is also supplied to the gL-liquid separator 5, and C111 etc. are precipitated in the gas-liquid separator 6 as a small P# bottle.
I! 1# The gold-forming gold-forming effect will be the highest in history.

The operating conditions for heat exchanger #4 and t-liquid reactor 6 were briefly touched upon earlier, but j! Add supplementary explanation. @Figure 8 is Moouni V brown legs (moisture 12, ash 4, I
IIM/stone foot ratio a = 8.0), temperature and decomposition production Co! ! This is a graph showing the relationship between CO
2 is burned after passing 200℃, and after that /7i! Separation from the kernels increases rapidly as the temperature rises, and at this stage there is sufficient moisture due to the dehydration process.

From this point of view, the following Kjl! It is recommended that all cropping conditions be met. That is, in the above description, when the temperature in the heat exchanger 4 is 250° C., it is said that the amount of decomposed CO21t;r is extremely small as shown in FIG. Therefore, as shown in Figure 1, it becomes necessary to supply CO2 from outside the prefecture. Therefore, if the system is to be covered by CO2, it is necessary to recite the temperature at nearly 400°C. That is, it is desirable that Cth, etc. 1) 1) be separated from the stone return structure, and the temperature at which the hexapods do not dissolve much, or below the boiling point of the slurry forming phase fII agent/! This is a one degree condition. The pressure is desirably set to 10 l1ir4 lower than the work efficiency of recompression when recovering steam.

FIG. 2 is a diagram showing an embodiment 70 for further improving the thermal efficiency in the heat exchanger 4. The electrolyte separator is divided into two stages of 6 m and 5b, the former 5a separates only steam, and the latter 5b is #I2# all precipitated. That is, in the example shown in Fig. 1, gcogas is installed to separate steam and COR, but it is difficult to completely separate the two, and thousands of C02 are mixed into the steam supplied to the heat exchanger 4. are doing.

Therefore, the thermal movement 1s#i in the heat exchanger 4 is not necessarily sufficient. Part 1 2 #I! ! In J, gas-liquid separator 5a
The plant is operated at extremely low internal pressure to suppress the decomposition of CO2, and the supply of cog to previous processes is discontinued. Therefore, #'iCOg is not mixed in the steam separated from the 9jt liquid fraction laml, and the COg is removed.
It is sufficient to supply it to heat exchanger #4 by simply pressurizing the necessary liquid through two vessels.Then, the *20gL liquid #1 vessel 6b is overheated to the pyrolysis temperature using a high-temperature heating medium, and the mixture is removed by decogmg. A small amount of steam is condensed and separated using a method such as the wafer method, and the condensed steam is treated as wastewater by harsh means.

CO produced by pyrolysis in 1M9tM separator bb
Hatake immediately reacts with (, a, etc. to form leg acid wood, so
The Cog mentioned above is an unreacted Cog, and this is IfiIEN.
I separator 5b [can be recycled. Therefore, although Figure 11 also shows the supply lines of COg outside the system, it is hardly necessary in the recruitment work.

Since the present invention was developed in the 1st century, the moisture and (a) contained in lignite are almost certainly treated prior to the hydrogenation and liquefaction reaction, and the moisture is released outside the system. With (
A, etc. become stable and delicate podates and cause blockage accidents. Therefore, it has become possible to perform extraction hydrogenation and liquefaction operations for browning stably for a long period of time. .

[Brief explanation of drawings]

FIG. 1.2 is a flow diagram of the embodiment, and FIG. 8 is a graph showing the relationship between decomposed CO2 and temperature. 4... Heat exchanger 6... Electrolyte separator 6...
COg removal device 8...Pressurizing means Applicant: Kobe Steel, Ltd. Continued from page 1 ■Applicant: Mitsubishi Chemical Industries, Ltd. 2-5-2 Marunouchi, Chiyoda-ku, Tokyo ■Applicant: Asia Oil Co., Ltd. 2-1 Uchisaiwai-cho, Chiyoda-ku, Tokyo No. 1 Procedure Amendment (-issued) 1986! Month! b Nippon Selection O Heating Dehydration Method 3, Relationship with the Amendment Case Patent Applicant Address No. 18, Wakihama-cho, Chuo-ku, Kobe City Name (119) Kokichi Takahashi 4, Representative of Kobe Steel, Ltd. , Agent Postal code: 530 Address: 2-3-7 Dojima, Kita-ku, Osaka City Shinko Building Kiyoshi III and Dai-Gyoen are also replaced with O in Attachment O.

Claims (1)

[Claims] (1) Prior to the hydrogenation and liquefaction reaction of the raw material slurry made by mixing raw brown leg and a solvent, the slurry is heated and pressurized, and if &
In a lignite dehydration method in which steam electricity that can be separated by fractionation is used as a heat source for raising the temperature, ω2-containing gas and/or outside the system generated due to gas-liquid separation in the dehydration step)
Heating of lignite, characterized in that the COQO gas to be supplied is blown into the slurry during the temperature and pressure raising step or the electrolyte separation step to precipitate O-leg mill-forming metal components in lignite as we#mill. Dehydration method. (2. In claim 1, the raw material slurry is overheated and supplied to a gas-liquid separator, and CO g
A heating dehydration method for lignite, in which the C0g-containing gas is injected into the slurry during a temperature and pressure raising step or a gas-liquid separation step after separating the gas contained therein. 1$141 In claim 51111, the gas-liquid separation process! JIITK separation, alIO gas-liquid separation is performed at a relatively low temperature side, so that it can be used as a separation factory for mainly water vapor. A heating dehydration method in which the C0g-containing gas obtained in the latter is blown into the raw material slurry during the gas-liquid separation step of II2.