CN105233819A - Reactivation method of palladium-carbon catalyst for producing disproportionated rosin - Google Patents

Abstract

The invention discloses a reactivation method of a palladium-carbon catalyst for producing disproportionated rosin and belongs to the technical field of producing disproportionated rosin. The method includes the steps of performing alkalization with addition of alkali, adding ethyl acetate into a reactor for two times continuously, stirring the mixture and allowing the mixture to stand, pouring clear supernate away, adding soft water, stirring and filtering the liquid, washing a filter residue and drying the filter residue, calcining the filter residue, and feeding hydrogen to perform a reduction reaction. The method can recover the catalytic activity of the palladium-carbon catalyst.

Description

The rejuvenation method of disproportionated rosin preparation palladium-carbon catalyst

Technical field

The invention belongs to disproportionated rosin preparing technical field, particularly relate to a kind of rejuvenation method of disproportionated rosin preparation palladium-carbon catalyst.

Background technology

Take rosin as raw material, with in the process of palladium carbon for catalyst preparing disproportionated rosin, often because the Impurity depositions such as the hot conditions of preparation process and organic materials are in reasons such as palladium-carbon catalyst surfaces, palladium-carbon catalyst activity is caused to reduce, even inactivation, make to react the palladium-carbon catalyst terminating rear recovery cannot continue to use, can only by dead catalyst burn become palladium ash more further regeneration process, thus add the consumption of palladium-carbon catalyst, improve the preparation cost of disproportionated rosin, also result in very large waste simultaneously.For this reason, people attempt the resurrection palladium-carbon catalyst reclaimed after use being carried out catalytic activity, make it be re-used.

Summary of the invention

The technical problem that the present invention solves is to provide a kind of rejuvenation method of disproportionated rosin preparation palladium-carbon catalyst, and this rejuvenation method can solve the problem of reacting the palladium-carbon catalyst terminating rear recovery and cannot continue to use.

In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:

It comprises the following steps:

A, the pending palladium-carbon catalyst of 0.8 weight portion ~ 1.0 weight portion is put into reactor, adding 0.2 weight portion ~ 0.4 weight portion concentration is the sodium hydroxide solution of 15%, be under the condition of 50 DEG C ~ 70 DEG C in temperature, alkalize 2 hours ~ 6 hours, then spend deionized water to neutral;

B, the ethyl acetate of the palladium-carbon catalyst after step A process and 0.8 weight portion ~ 1.0 weight portion is put into reactor, be stir 30 minutes ~ 60 minutes under the condition of 50 DEG C ~ 70 DEG C in temperature, then stop stirring, leave standstill 20 hours ~ 24 hours, remove upper strata settled solution;

After C, step B, in described reactor, add the ethyl acetate of 0.8 weight portion ~ 1.0 weight portion, stir 10 minutes ~ 20 minutes at normal temperatures, then stop stirring, leave standstill 6 hours ~ 8 hours, remove upper strata settled solution;

After D, step C, in described reactor, add the soft water of 0.8 weight portion ~ 1.0 weight portion, stir 20 minutes ~ 30 minutes at the temperature of 80 DEG C ~ 100 DEG C, then stop stirring, filter, the filter residue soft water obtained is washed 3 times ~ 5 times;

After E, D step, first the filter residue after washing is dried at 50 DEG C ~ 70 DEG C, and then calcine 1 hour ~ 3 hours at 400 DEG C ~ 900 DEG C, finally pass into the hydrogen that purity is 99.5%, reduce 4 hours ~ 6 hours at 200 DEG C ~ 220 DEG C, obtained.

Owing to adopting technique scheme, the beneficial effect that the present invention obtains is:

The present invention can effectively remove the impurity being deposited on palladium-carbon catalyst surface, readjust the deployment conditions of palladium at activated carbon surface, solve the temporary inactivation of palladium-carbon catalyst or the active problem reduced, recover the catalytic activity of inactivation palladium-carbon catalyst largely or improve the catalytic activity of the active palladium-carbon catalyst reduced.

Detailed description of the invention

Below in conjunction with specific embodiment, the invention will be further described, and protection scope of the present invention is not only confined to following examples.

Embodiment 1

The rejuvenation method of this disproportionated rosin preparation palladium-carbon catalyst comprises the following steps:

A, pending for 0.8kg palladium-carbon catalyst is put into reactor, adding the sodium hydroxide solution that 0.4kg concentration is 15%, is under the condition of 50 DEG C in temperature, alkalizes 6 hours, then spends deionized water to neutral;

B, the palladium-carbon catalyst after step A process and 1.0kg ethyl acetate are put into reactor, be stir 60 minutes under the condition of 50 DEG C in temperature, then stop stirring, leave standstill 20 hours, remove upper strata settled solution;

After C, step B, in described reactor, add 1.0kg ethyl acetate, stir 10 minutes at normal temperatures, then stop stirring, leave standstill 8 hours, remove upper strata settled solution;

After D, step C, in described reactor, add 1.0kg soft water, stir 30 minutes at the temperature of 80 DEG C, then stop stirring, filter, the filter residue soft water obtained is washed 3 times;

After E, D step, first the filter residue after washing is dried at 50 DEG C, and then calcine 3 hours at 400 DEG C, finally pass into the hydrogen that purity is 99.5%, reduce 6 hours at 200 DEG C, obtained.

Embodiment 2

The rejuvenation method of this disproportionated rosin preparation palladium-carbon catalyst comprises the following steps:

A, pending for 1.0kg palladium-carbon catalyst is put into reactor, adding the sodium hydroxide solution that 0.2kg concentration is 15%, is under the condition of 70 DEG C in temperature, alkalizes 2 hours, then spends deionized water to neutral;

B, the palladium-carbon catalyst after step A process and 0.8kg ethyl acetate are put into reactor, be stir 30 minutes under the condition of 70 DEG C in temperature, then stop stirring, leave standstill 24 hours, remove upper strata settled solution;

After C, step B, in described reactor, add 0.8kg ethyl acetate, stir 20 minutes at normal temperatures, then stop stirring, leave standstill 6 hours, remove upper strata settled solution;

After D, step C, in described reactor, add 0.8kg soft water, stir 20 minutes at the temperature of 100 DEG C, then stop stirring, filter, the filter residue soft water obtained is washed 5 times;

After E, D step, first the filter residue after washing is dried at 70 DEG C, and then calcine 1 hour at 900 DEG C, finally pass into the hydrogen that purity is 99.5%, reduce 4 hours at 220 DEG C, obtained.

Embodiment 3

The rejuvenation method of this disproportionated rosin preparation palladium-carbon catalyst comprises the following steps:

A, pending for 0.9kg palladium-carbon catalyst is put into reactor, adding the sodium hydroxide solution that 0.3kg concentration is 15%, is under the condition of 60 DEG C in temperature, alkalizes 4 hours, then spends deionized water to neutral;

B, the palladium-carbon catalyst after step A process and 0.9kg ethyl acetate are put into reactor, be stir 45 minutes under the condition of 60 DEG C in temperature, then stop stirring, leave standstill 22 hours, remove upper strata settled solution;

After C, step B, in described reactor, add 0.9kg ethyl acetate, stir 15 minutes at normal temperatures, then stop stirring, leave standstill 7 hours, remove upper strata settled solution;

After D, step C, in described reactor, add 0.9kg soft water, stir 25 minutes at the temperature of 95 DEG C, then stop stirring, filter, the filter residue soft water obtained is washed 4 times;

After E, D step, first the filter residue after washing is dried at 60 DEG C, and then calcine 2 hours at 700 DEG C, finally pass into the hydrogen that purity is 99.5%, reduce 5 hours at 210 DEG C, obtained.

The catalytic activity that embodiment 1 ~ 3 is brought back to life the palladium-carbon catalyst obtained, original new palladium-carbon catalyst and both mixtures is tested, and its result is as table 1.

Table 1

As can be seen from above-mentioned table 1, the present invention effectively can recover the catalytic activity of inactivation or the active palladium-carbon catalyst reduced; The present invention brings back to life the palladium-carbon catalyst obtained and palladium-carbon catalyst that part is new can be replaced in the preparation process of disproportionated rosin, thus decreases the consumption of new palladium-carbon catalyst, reduces its preparation cost.

Claims (1)

1. a rejuvenation method for disproportionated rosin preparation palladium-carbon catalyst, is characterized in that comprising the following steps:

A, the pending palladium-carbon catalyst of 0.8 weight portion ~ 1.0 weight portion is put into reactor, adding 0.2 weight portion ~ 0.4 weight portion concentration is the sodium hydroxide solution of 15%, be under the condition of 50 DEG C ~ 70 DEG C in temperature, alkalize 2 hours ~ 6 hours, then spend deionized water to neutral;

B, the ethyl acetate of the palladium-carbon catalyst after step A process and 0.8 weight portion ~ 1.0 weight portion is put into reactor, be stir 30 minutes ~ 60 minutes under the condition of 50 DEG C ~ 70 DEG C in temperature, then stop stirring, leave standstill 20 hours ~ 24 hours, remove upper strata settled solution;

After C, step B, in described reactor, add the ethyl acetate of 0.8 weight portion ~ 1.0 weight portion, stir 10 minutes ~ 20 minutes at normal temperatures, then stop stirring, leave standstill 6 hours ~ 8 hours, remove upper strata settled solution;

After D, step C, in described reactor, add the soft water of 0.8 weight portion ~ 1.0 weight portion, stir 20 minutes ~ 30 minutes at the temperature of 80 DEG C ~ 100 DEG C, then stop stirring, filter, the filter residue soft water obtained is washed 3 times ~ 5 times;

After E, D step, first the filter residue after washing is dried at 50 DEG C ~ 70 DEG C, and then calcine 1 hour ~ 3 hours at 400 DEG C ~ 900 DEG C, finally pass into the hydrogen that purity is 99.5%, reduce 4 hours ~ 6 hours at 200 DEG C ~ 220 DEG C, obtained.